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Sample records for plasma multiple-collector mass

  1. Matrix effects of calcium on high-precision sulfur isotope measurement by multiple-collector inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Liu, Chenhui; Bian, Xiao-Peng; Yang, Tao; Lin, An-Jun; Jiang, Shao-Yong

    2016-05-01

    Multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) has been successfully applied in the rapid and high-precision measurement for sulfur isotope ratios in recent years. During the measurement, the presence of matrix elements would affect the instrumental mass bias for sulfur and these matrix-induced effects have aroused a lot of researchers' interest. However, these studies have placed more weight on highlighting the necessity for their proposed correction protocols (e.g., chemical purification and matrix-matching) while less attention on the key property of the matrix element gives rise to the matrix effects. In this study, four groups of sulfate solutions, which have different concentrations of sulfur (0.05-0.60mM) but a constant sequence of atomic calcium/sulfur ratios (0.1-50), are investigated under wet (solution) and dry (desolvation) plasma conditions to make a detailed evaluation on the matrix effects from calcium on sulfur isotope measurement. Based on a series of comparative analyses, we indicated that, the matrix effects of calcium on both measured sulfur isotope ratios and detected (32)S signal intensities are dependent mainly on the absolute calcium concentration rather than its relative concentration ratio to sulfur (i.e., atomic calcium/sulfur ratio). Also, for the same group of samples, the matrix effects of calcium under dry plasma condition are much more significant than that of wet plasma. This research affords the opportunity to realize direct and relatively precise sulfur isotope measurement for evaporite gypsum, and further provides some suggestions with regard to sulfur isotope analytical protocols for sedimentary pore water.

  2. Rapid lead isotope analysis of archaeological metals by multiple-collector inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Baker, J.A.; Stos, S.; Waight, Tod Earle

    2006-01-01

    Lead isotope ratios in archaeological silver and copper were determined by MC-ICPMS using laser ablation and bulk dissolution without lead purification. Laser ablation results on high-lead metals and bulk solution analyses on all samples agree within error of TIMS data, suggesting that problems...... from isobaric interferences and/or mass bias variations due to the presence of matrix elements are insignificant. Inaccurate laser ablation analyses on low-lead copper reflect erroneous mass bias corrections from use of a non-matrix matched standard. However, in most cases, silver and copper...... are analysable for lead isotopes by bulk dissolution or laser ablation MC-ICPMS with simplified sample preparation....

  3. Evaluation of lead isotope compositions of NIST NBS 981 measured by thermal ionization mass spectrometer and multiple-collector inductively coupled plasma mass spectrometer

    Directory of Open Access Journals (Sweden)

    Honglin Yuan

    2016-09-01

    Full Text Available Because Pb isotopes can be used for tracing, they are widely used in many disciplines. The detection and analysis of Pb isotopes of bulk samples are usually conducted using thermal ionization mass spectrometer (TIMS and multiple-collector inductively coupled plasma mass spectrometer (MC-ICP-MS, both of which need external reference materials with known isotopic compositions to correct for the mass discrimination effect produced during analysis. NIST NBS 981 is the most widely used reference material for Pb isotope analysis; however, the isotopic compositions reported by various analytical laboratories, especially those using TIMS, vary from each other. In this study, we statistically evaluated 229 reported TIMS analysis values collected by GeoReM in the last 30 years, 176 reported MC-ICP-MS analysis values, and 938 MC-ICP-MS analysis results from our laboratory in the last five years. After careful investigation, only 40 TIMS results were found to have double or triple spikes. The ratios of the overall weighted averages, 206Pb/204Pb, 207Pb/204Pb, and 208Pb/204Pb, obtained from 40 spiked TIMS reports and 1114 MC-ICP-MS results of NIST NBS 981 isotopes were 16.9406 ± 0.0003 (2s, 15.4957 ± 0.0002 (2s, and 36.7184 ± 0.0007 (2s, respectively.

  4. Development of an on-line flow injection Sr/matrix separation method for accurate, high-throughput determination of Sr isotope ratios by multiple collector-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Galler, Patrick; Limbeck, Andreas; Boulyga, Sergei F; Stingeder, Gerhard; Hirata, Takafumi; Prohaska, Thomas

    2007-07-01

    This work introduces a newly developed on-line flow injection (FI) Sr/Rb separation method as an alternative to the common, manual Sr/matrix batch separation procedure, since total analysis time is often limited by sample preparation despite the fast rate of data acquisition possible by inductively coupled plasma-mass spectrometers (ICPMS). Separation columns containing approximately 100 muL of Sr-specific resin were used for on-line FI Sr/matrix separation with subsequent determination of (87)Sr/(86)Sr isotope ratios by multiple collector ICPMS. The occurrence of memory effects exhibited by the Sr-specific resin, a major restriction to the repetitive use of this costly material, could successfully be overcome. The method was fully validated by means of certified reference materials. A set of two biological and six geological Sr- and Rb-bearing samples was successfully characterized for its (87)Sr/(86)Sr isotope ratios with precisions of 0.01-0.04% 2 RSD (n = 5-10). Based on our measurements we suggest (87)Sr/(86)Sr isotope ratios of 0.713 15 +/- 0.000 16 (2 SD) and 0.709 31 +/- 0.000 06 (2 SD) for the NIST SRM 1400 bone ash and the NIST SRM 1486 bone meal, respectively. Measured (87)Sr/(86)Sr isotope ratios for five basalt samples are in excellent agreement with published data with deviations from the published value ranging from 0 to 0.03%. A mica sample with a Rb/Sr ratio of approximately 1 was successfully characterized for its (87)Sr/(86)Sr isotope signature to be 0.718 24 +/- 0.000 29 (2 SD) by the proposed method. Synthetic samples with Rb/Sr ratios of up to 10/1 could successfully be measured without significant interferences on mass 87, which would otherwise bias the accuracy and uncertainty of the obtained data.

  5. High-accuracy determination of iron in seawater by isotope dilution multiple collector inductively coupled plasma mass spectrometry (ID-MC-ICP-MS) using nitrilotriacetic acid chelating resin for pre-concentration and matrix separation

    Energy Technology Data Exchange (ETDEWEB)

    Jong, Jeroen de [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Unite Isotopes: Petrologie et Environnement - IPE CP 160/02, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium)], E-mail: jdejong@ulb.ac.be; Schoemann, Veronique [Universite Libre de Bruxelles (ULB), Ecologie des Systemes Aquatiques (ESA) CP 221, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium); Lannuzel, Delphine [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Laboratoire d' Oceanographie Chimique et Geochimie des Eaux - LOCGE CP 208, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium); Tison, Jean-Louis [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Laboratoire de Glaciologie - GLACIOL CP 160/03, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium); Mattielli, Nadine [Universite Libre de Bruxelles (ULB), Departement des Sciences de la Terre et de l' Environnement (DSTE), Unite Isotopes: Petrologie et Environnement - IPE CP 160/02, Avenue F.D. Roosevelt 50, B-1050 Brussels (Belgium)

    2008-08-15

    In the present paper we describe a robust and simple method to measure dissolved iron (DFe) concentrations in seawater down to <0.1 nmol L{sup -1} level, by isotope dilution multiple collector inductively coupled plasma mass spectrometry (ID-MC-ICP-MS) using a {sup 54}Fe spike and measuring the {sup 57}Fe/{sup 54}Fe ratio. The method provides for a pre-concentration step (100:1) by micro-columns filled with the resin NTA Superflow of 50 mL seawater samples acidified to pH 1.9. NTA Superflow is demonstrated to quantitatively extract Fe from acidified seawater samples at this pH. Blanks are kept low (grand mean 0.045 {+-} 0.020 nmol L{sup -1}, n = 21, 3x S.D. limit of detection per session 0.020-0.069 nmol L{sup -1} range), as no buffer is required to adjust the sample pH for optimal extraction, and no other reagents are needed than ultrapure nitric acid, 12 mM H{sub 2}O{sub 2}, and acidified (pH 1.9) ultra-high purity (UHP) water. We measured SAFe (sampling and analysis of Fe) reference seawater samples Surface-1 (0.097 {+-} 0.043 nmol L{sup -1}) and Deep-2 (0.91 {+-} 0.17 nmol L{sup -1}) and obtained results that were in excellent agreement with their DFe consensus values: 0.118 {+-} 0.028 nmol L{sup -1} (n = 7) for Surface-1 and 0.932 {+-} 0.059 nmol L{sup -1} (n = 9) for Deep-2. We also present a vertical DFe profile from the western Weddell Sea collected during the Ice Station Polarstern (ISPOL) ice drift experiment (ANT XXII-2, RV Polarstern) in November 2004-January 2005. The profile shows near-surface DFe concentrations of {approx}0.6 nmol L{sup -1} and bottom water enrichment up to 23 nmol L{sup -1} DFe.

  6. Platinum stable isotope ratio measurements by double-spike multiple collector ICPMS

    DEFF Research Database (Denmark)

    Creech, J.; Baker, J.; Handler, M.

    2013-01-01

    external element (Pb) doping to correct for instrumental mass bias and have identified relative Pt isotope differences of up to 10% from the reference values for this standard. The new isotopic composition of the IRMM-010 standard (Pt = 0.01289%, Pt = 0.7938%, Pt = 32.81%, Pt = 33.79%, Pt = 25.29% and Pt......We present a new technique for the precise determination of platinum (Pt) stable isotope ratios by multiple-collector inductively coupled plasma mass spectrometry (MC-ICPMS) using two different Pt double-spikes ( Pt-Pt and Pt-Pt). Results are expressed relative to the IRMM-010 Pt isotope standard......) can be obtained on Pt stable isotope ratios with either double-spike. Elemental doping tests reveal that double-spike corrected Pt stable isotope ratios are insensitive to the presence of relatively high (up to 10%) levels of matrix elements, although the Pt-Pt double-spike is affected by an isobaric...

  7. 多接收器电感耦合等离子体质谱的新应用%New Application of Multiple Collector ICPMS

    Institute of Scientific and Technical Information of China (English)

    Nick Belshaw

    2007-01-01

    Advances in Inorganic Geochemistry have often been dependant on introduction of new technology. The development of Inductively Coupled Plasma Mass Spectrometry (ICPMS) has allowed high-precision isotopic analysis of elements previously very difficult to analyse. In Oxford we have invested heavily in Multiple Collector Plasma Mass Spectrometry to address problems ranging from Cosmic to Environmental Chemistry. Examples of current projects being pursued are an investigation of Cr-isotopes to identify a possible impact event at the Jurassic-Triassic boundary, and the use of U-series isotopes in Oceanography.%无机地球化学研究的进展通常依赖于新的技术开发.电感耦合等离子体质谱(ICP-MS)技术可以进行高精度的同位素比值分析,使以前很难测定的元素的分析成为可能.牛津大学地球科学系已经越来越多地开展多接收器电感耦合等离子体质谱分析,着重于解决从宇宙至环境化学领域的诸多问题.目前主要研究Cr同位素,确定Cr对Jurassic-Triassic边界可能产生的影响事件,以及采用铀系列同位素进行海洋学研究.

  8. 多接收器电感耦合等离子质谱精确测定钕同位素组成%Accurate Measurement of Neodymium Isotopic Composition Using Neptune Multiple Collector Inductively Coupled Plasma Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    杨岳衡; 张宏福; 谢烈文; 吴福元

    2007-01-01

    报道了本实验室近两年来Neptune MC-ICP-MS测试Nd同位素的结果.测试结果显示样品化学分离中伴随的大量铈对钕同位素组成测定没有影响;而分离后残余少量钐,在一定范围内(钐/钕<0.04)可以直接扣除,获得准确的Nd同位素组成.Neptune MC-ICP-MS和热电离质谱(TIMS)平行测定实际地质样品表明,Neptune MC-ICP-MS可以精确测定Nd同位素组成,与经典的TIMS技术相比,MC-ICP-MS可以获得与TIMS相媲美的数据精度,而且分析时间缩短,效率明显提高.

  9. Accurate Measurement of Strontium Isotopic Composition by Neptune Multiple Collector Inductively Coupled Plasma Mass Spectrometry%Neptune多接收器等离子体质谱精确测定锶同位素组成

    Institute of Scientific and Technical Information of China (English)

    杨岳衡; 张宏福; 吴福元; 谢烈文; 张艳斌

    2005-01-01

    报道了近两年来在Neptune多接收器等离子体质谱(MC-ICP-MS)上对NIST SRM987的测试结果.针对实际地质样品,Neptune MC-ICP-MS和热电离质谱(TIMS)进行了平行测定.Neptune MC-ICP-MS可以精确测定锶同位素组成,与传统的TIMS相比,MC-ICP-MS可以获得与TIMS相媲美的数据精度,而且分析时间短,效率高.对于等离子体载气--氩气中少量氪的干扰,可以直接扣除;对于样品中少量铷(Rb/Sr<0.01)的干扰,同样可以直接扣除,从而获得准确的锶同位素组成.

  10. Plasma Mass Filters For Nuclear Waste Reprocessing

    Energy Technology Data Exchange (ETDEWEB)

    Fetterman, Abraham J. [Princeton Plasma Physics Lab. (PPPL), Princeton, NJ (United States); Fisch, Nathaniel J. [Princeton Plasma Physics Lab. (PPPL), Princeton, NJ (United States)

    2011-05-01

    Practical disposal of nuclear waste requires high-throughput separation techniques. The most dangerous part of nuclear waste is the fission product, which contains the most active and mobile radioisotopes and produces most of the heat. We suggest that the fission products could be separated as a group from nuclear waste using plasma mass filters. Plasmabased processes are well suited to separating nuclear waste, because mass rather than chemical properties are used for separation. A single plasma stage can replace several stages of chemical separation, producing separate streams of bulk elements, fission products, and actinoids. The plasma mass filters may have lower cost and produce less auxiliary waste than chemical processing plants. Three rotating plasma configurations are considered that act as mass filters: the plasma centrifuge, the Ohkawa filter, and the asymmetric centrifugal trap.

  11. Plasma Mass Filters For Nuclear Waste Reprocessing

    Energy Technology Data Exchange (ETDEWEB)

    Abraham J. Fetterman and Nathaniel J. Fisch

    2011-05-26

    Practical disposal of nuclear waste requires high-throughput separation techniques. The most dangerous part of nuclear waste is the fission product, which contains the most active and mobile radioisotopes and produces most of the heat. We suggest that the fission products could be separated as a group from nuclear waste using plasma mass filters. Plasmabased processes are well suited to separating nuclear waste, because mass rather than chemical properties are used for separation. A single plasma stage can replace several stages of chemical separation, producing separate streams of bulk elements, fission products, and actinoids. The plasma mass filters may have lower cost and produce less auxiliary waste than chemical processing plants. Three rotating plasma configurations are considered that act as mass filters: the plasma centrifuge, the Ohkawa filter, and the asymmetric centrifugal trap.

  12. Plasma source mass spectrometry in experimental nutrition.

    Science.gov (United States)

    Barnes, R M

    1998-01-01

    The development and commercial availability of plasma ion source, specifically inductively coupled plasma, mass spectrometers (ICP-MS) have significantly extended the potential application of stable isotopes for nutritional modeling. The status of research and commercial ICP-MS instruments, and their applications and limitations for stable isotopic studies are reviewed. The consequences of mass spectroscopic resolution and measurement sensitivity obtainable with quadrupole, sector, time-of-flight, and trap instruments on stable isotope analysis are examined. Requirements for reliable isotope measurements with practical biological samples including tissues and fluids are considered. The possibility for stable isotope analysis in chemically separated compounds (speciation) also is explored. On-line compound separations by chromatography or electrophoresis, for example, have been combined instrumentally with ICP-MS. Som possibilities and requirements are described for stable isotope speciation analysis.

  13. Numerical analysis of the EHD driven flow with heat transfer in a smooth channel using multiple collectors

    Science.gov (United States)

    Taghavi Fadaki, S. S.; Amanifard, N.; Deylami, H. M.; Dolati, F.

    2017-02-01

    In the present study, a new design of collecting electrodes is studied for performing a higher performance in EHD phenomena in a smooth channel. The effect of the electric field on the heat transfer enhancement and swirling flow patterns for a new design of multiple collectors in a smooth channel is numerically investigated with 2-D approach. In this regard, the corona device configuration comprises a single fixed emitting wire situated at the centerline of the channel and different grounded electrode arrangements which are in two types of wire and plate. The results indicate that the multi-collector arrangements cause significant changes in the flow pattern, heat transfer coefficient and friction factor. Furthermore, it is found that the thermal enhancement factor has remarkable growth, and EHD efficiency for two types of wire and plate collectors is notable. Besides, as an outstanding result, the electrohydrodynamic phenomenon has a negative effect on the heat transfer enhancement depending upon the values of Reynolds number and applied electric potential.

  14. Physical properties of erupting plasma associated with coronal mass ejections

    Science.gov (United States)

    Lee, J.; Raymond, J. C.; Reeves, K. K.; Moon, Y.; Kim, K.

    2013-12-01

    We investigate the physical properties (temperature, density, and mass) of erupting plasma observed in X-rays and EUV, which are all associated with coronal mass ejections observed by SOHO/LASCO. The erupting plasmas are observed as absorption or emission features in the low corona. The absorption feature provides a lower limit to the cold mass while the emission feature provides an upper limit to the mass of observed plasma in X-ray and EUV. We compare the mass constraints for each temperature response and find that the mass estimates in EUV and XRT are smaller than the total mass in the coronagraph. Several events were observed by a few passbands in the X-rays, which allows us to determine the temperature of the eruptive plasma using a filter ratio method. The temperature of one event is estimated at about 8.6 MK near the top of the erupting plasma. This measurement is possibly an average temperature for higher temperature plasma because the XRT is more sensitive at higher temperatures. In addition, a few events show that the absorption features of a prominence or a loop change to emission features with the beginning of their eruptions in all EUV wavelengths of SDO/AIA, which indicates the heating of the plasma. By estimating the physical properties of the erupting plasmas, we discuss the heating of the plasmas associated with coronal mass ejections in the low corona.

  15. Ion sampling and transport in Inductively Coupled Plasma Mass Spectrometry

    Science.gov (United States)

    Farnsworth, Paul B.; Spencer, Ross L.

    2017-08-01

    Quantitative accuracy and high sensitivity in inductively coupled plasma mass spectrometry (ICP-MS) depend on consistent and efficient extraction and transport of analyte ions from an inductively coupled plasma to a mass analyzer, where they are sorted and detected. In this review we examine the fundamental physical processes that control ion sampling and transport in ICP-MS and compare the results of theory and computerized models with experimental efforts to characterize the flow of ions through plasma mass spectrometers' vacuum interfaces. We trace the flow of ions from their generation in the plasma, into the sampling cone, through the supersonic expansion in the first vacuum stage, through the skimmer, and into the ion optics that deliver the ions to the mass analyzer. At each stage we consider idealized behavior and departures from ideal behavior that affect the performance of ICP-MS as an analytical tool.

  16. Plasma Viscosity with Mass Transport in Spherical ICF Implosion Simulations

    CERN Document Server

    Vold, Erik L; Ortega, Mario I; Moll, Ryan; Fenn, Daniel; Molvig, Kim

    2015-01-01

    The effects of viscosity and small-scale atomic-level mixing on plasmas in inertial confinement fusion (ICF) currently represent challenges in ICF research. Many current ICF hydrodynamic codes ignore the effects of viscosity though recent research indicates viscosity and mixing by classical transport processes may have a substantial impact on implosion dynamics. We have implemented a Lagrange hydrodynamic code in one-dimensional spherical geometry with plasma viscosity and mass transport and including a three temperature model for ions, electrons, and radiation treated in a gray radiation diffusion approximation. The code is used to study ICF implosion differences with and without plasma viscosity and to determine the impacts of viscosity on temperature histories and neutron yield. It was found that plasma viscosity has substantial impacts on ICF shock dynamics characterized by shock burn timing, maximum burn temperatures, convergence ratio, and time history of neutron production rates. Plasma viscosity reduc...

  17. Imaging thermal plasma mass and velocity analyzer

    Science.gov (United States)

    Yau, Andrew W.; Howarth, Andrew

    2016-07-01

    We present the design and principle of operation of the imaging ion mass and velocity analyzer on the Enhanced Polar Outflow Probe (e-POP), which measures low-energy (1-90 eV/e) ion mass composition (1-40 AMU/e) and velocity distributions using a hemispherical electrostatic analyzer (HEA), a time-of-flight (TOF) gate, and a pair of toroidal electrostatic deflectors (TED). The HEA and TOF gate measure the energy-per-charge and azimuth of each detected ion and the ion transit time inside the analyzer, respectively, providing the 2-D velocity distribution of each major ionospheric ion species and resolving the minor ion species under favorable conditions. The TED are in front of the TOF gate and optionally sample ions at different elevation angles up to ±60°, for measurement of 3-D velocity distribution. We present examples of observation data to illustrate the measurement capability of the analyzer, and show the occurrence of enhanced densities of heavy "minor" O++, N+, and molecular ions and intermittent, high-velocity (a few km/s) upward and downward flowing H+ ions in localized regions of the quiet time topside high-latitude ionosphere.

  18. Plasma Heating Suring a Coronal Mass Ejection Observed by SOHO

    CERN Document Server

    Murphy, N A; Korreck, K E

    2011-01-01

    We perform a time-dependent ionization analysis to constrain plasma heating requirements during a fast partial halo coronal mass ejection (CME) observed on 2000 June 28 by the Ultraviolet Coronagraph Spectrometer (UVCS) aboard the Solar and Heliospheric Observatory (SOHO). We use two methods to derive densities from the UVCS measurements, including a density sensitive O V line ratio at 1213.85 and 1218.35 Angstroms, and radiative pumping of the O VI 1032,1038 doublet by chromospheric emission lines. The most strongly constrained feature shows cumulative plasma heating comparable to or greater than the kinetic energy, while features observed earlier during the event show cumulative plasma heating comparable to or less than the kinetic energy. SOHO Michelson Doppler Imager (MDI) observations are used to estimate the active region magnetic energy. We consider candidate plasma heating mechanisms and provide constraints when possible. Because this CME was associated with a relatively weak flare, the contribution b...

  19. E × B ion mass spectroscopy in magnetised plasmas

    Science.gov (United States)

    Hellblom, K. G.; Armstrong, R. J.

    1995-02-01

    A spectrometer based on the E × B drift during the transit time of the ion through a cross field region has been tested in a hydrogen plasma in the Blaamann toroidal plasma device [T. Brundtland, Vacuum 43 (1992) 185]. The magnetic field B, is the field of the device. The electric field E, which is imposed and oriented perpendicular to the magnetic field, is swept with a time long compared to the ion transit time. The ions are accelerated along the magnetic field as they enters the cross field region giving them a velocity and a transit time proportional to the charge over the mass.

  20. SVSCf plasma desorption mass spectrometry: recent advances and applications

    Energy Technology Data Exchange (ETDEWEB)

    Kamensky, I.; Craig, A.G.

    1987-01-01

    SVSCf plasma desorption mass spectrometry (PDMS) as utilized in the BIO-ION instruments is described. The sensitivity of the technique is investigated for varying amounts of bovine insulin. The results show accurate mass assignment for pmole amounts of sample. Several methods, currently used for sample preparation in PDMS, are described. Spectra of the antibiotic nisin using two different sample preparation techniques show significant variation. The fragmentation pattern of reduced acetylated maltoheptaose is also presented. The initial results obtained using a new PDMS instrument equipped with variable flight path are shown. The increased resolution is illustrated using the extended flight path to measure the molecular ion region of the maltoheptaose.

  1. Measurement of the effective plasma ion mass in large tokamaks

    Energy Technology Data Exchange (ETDEWEB)

    Lister, J.B.; Villard, L.; Ridder, G. de [Ecole Polytechnique Federale, Lausanne (Switzerland). Centre de Recherche en Physique des Plasma (CRPP)

    1997-06-01

    There is not yet a straightforward method for the measurement of the D-T ratio in the centre of a tokamak plasma. One of the simpler measurements put forward in the past is the interpretation of the MHD spectrum in the frequency range of the Global Alfven Eigenmodes (GAE). However, the frequencies of these modes do not only depend on the plasma mass, but are also quite strongly dependent on the details of the current and density profiles, creating a problem of deconvolution of the estimate of the plasma mass from an implicit relationship between several measurable plasma parameters and the detected eigenmode frequencies. This method has been revised to assess its likely precision for the JET tokamak. The low n GAE modes are sometimes too close to the continuum edge to be detectable and the interpretation of the GAE spectrum is rendered less direct than had been hoped. We present a statistical study on the precision with which the D-T ratio could be estimated from the GAE spectrum on JET. (author) 4 figs., 8 refs.

  2. Modeling the chemistry of plasma polymerization using mass spectrometry.

    Science.gov (United States)

    Ihrig, D F; Stockhaus, J; Scheide, F; Winkelhake, Oliver; Streuber, Oliver

    2003-04-01

    The goal of the project is a solvent free painting shop. The environmental technologies laboratory is developing processes of plasma etching and polymerization. Polymerized thin films are first-order corrosion protection and primer for painting. Using pure acetylene we get very nice thin films which were not bonded very well. By using air as bulk gas it is possible to polymerize, in an acetylene plasma, well bonded thin films which are stable first-order corrosion protections and good primers. UV/Vis spectroscopy shows nitrogen oxide radicals in the emission spectra of pure nitrogen and air. But nitrogen oxide is fully suppressed in the presence of acetylene. IR spectroscopy shows only C=O, CH(2) and CH(3) groups but no nitrogen species. With the aid of UV/Vis spectra and the chemistry of ozone formation it is possible to define reactive traps and steps, molecule depletion and processes of proton scavenging and proton loss. Using a numerical model it is possible to evaluate these processes and to calculate theoretical mass spectra. Adjustment of theoretical mass spectra to real measurements leads to specific channels of polymerization which are driven by radicals especially the acetyl radical. The estimated theoretical mass spectra show the specific channels of these chemical processes. It is possible to quantify these channels. This quantification represents the mass flow through this chemical system. With respect to these chemical processes it is possible to have an idea of pollutant production processes.

  3. A Review on Inductively Coupled Plasma Mass Spectroscopy

    Directory of Open Access Journals (Sweden)

    Ramyalakshmi G

    2012-12-01

    Full Text Available Inductively coupled plasma mass spectroscopy is routinely used in many diverse research fields such as earth, environmental, life and forensic sciences and in food, material, chemical, semiconductor and nuclear industries. The high ion density and the high temperature in a plasma provide an ideal atomizer and element ionizer for all types of samples and materials introduced by a specialised devices .outstanding properties such as high sensitivity, relative salt tolerance, compound-independent element response and highest quantitation accuracy lead to the unchallenged performance of ICPMS in efficiently detecting, identifying and reliably quantifying trace element. The increasing availability of relevant reference compounds and high separation selectively extend the molecular identification capability of ICPMS hyphenated to species – specific separation techniques

  4. Plant Phosphoproteomics: Analysis of Plasma Membrane Transporters by Mass Spectrometry

    DEFF Research Database (Denmark)

    Ye, Juanying; Rudashevskaya, Elena; Young, Clifford

    important physiological functions, such as stomata aperture, cell elongation, or cellular pH regulation. It is known that the activity of plant plasma membrane H+-ATPase is regulated by phosphorylation. Therefore, we first investigated the phosphorylation profile of plant H+-ATPase by enriching...... the phosphopeptides with optimized TiO2 and IMAC enrichment methods prior to MS analysis. We further investigated the global phosphorylation profile of the whole plant plasma membrane proteins using the combination of our recently established phosphopeptide enrichment method, Calcium phosphate precipitation......  Phosphorylation is a key regulatory factor in all aspects of eukaryotic biology including the regulation of plant membrane-bound transport proteins. To date, mass spectrometry (MS) has been introduced as powerful technology for study of post translational modifications (PTMs), including protein...

  5. Quantitative aspects of inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Bulska, Ewa; Wagner, Barbara

    2016-10-01

    Accurate determination of elements in various kinds of samples is essential for many areas, including environmental science, medicine, as well as industry. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful tool enabling multi-elemental analysis of numerous matrices with high sensitivity and good precision. Various calibration approaches can be used to perform accurate quantitative measurements by ICP-MS. They include the use of pure standards, matrix-matched standards, or relevant certified reference materials, assuring traceability of the reported results. This review critically evaluates the advantages and limitations of different calibration approaches, which are used in quantitative analyses by ICP-MS. Examples of such analyses are provided. This article is part of the themed issue 'Quantitative mass spectrometry'.

  6. Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Baxter, Douglas C., E-mail: douglas.baxter@alsglobal.com [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Faarinen, Mikko [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Osterlund, Helene; Rodushkin, Ilia [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Division of Geosciences, Lulea University of Technology, 977 87 Lulea (Sweden); Christensen, Morten [ALS Scandinavia AB, Maskinvaegen 2, 183 53 Taeby (Sweden)

    2011-09-09

    Highlights: {center_dot} We determine methylmercury in serum and plasma using isotope dilution calibration. {center_dot} Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. {center_dot} Data for 50 specimens provides first reference range for methylmercury in serum. {center_dot} Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with {sup 198}Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) {mu}g L{sup -1} could be performed with uncertainty amplification factors <2. A limit of quantification of 0.03 {mu}g L{sup -1} was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were <10% at added concentration levels of 0.14 {mu}g L{sup -1}, 0.35 {mu}g L{sup -1} and 2.8 {mu}g L{sup -1}, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; <0.03-0.19) {mu}g L{sup -1}. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

  7. Plasma Desorption Mass Spectrometry analysis of HCOOH ice

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, D.P.P.; Rocco, M.L.M. [Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Federal do Rio de Janeiro, Cidade Universitaria, Ilha do Fundao, 21949-900 Rio de Janeiro, RJ (Brazil); Boechat-Roberty, H.M. [Observatorio do Valongo, Universidade Federal do Rio de Janeiro, Ladeira Pedro Antonio, 43, Centro, Rio de Janeiro, RJ (Brazil); Iza, P.; Martinez, R. [Departamento de Fisica, Pontificia Universidade Catolica do Rio de Janeiro, 22543-900 Rio de Janeiro (Brazil); Homem, M.G.P. [Laboratorio Nacional de Luz Sincrotron (LNLS), Box 6192, 13084-971 Campinas, SP (Brazil); Silveira, E.F. da [Departamento de Fisica, Pontificia Universidade Catolica do Rio de Janeiro, 22543-900 Rio de Janeiro (Brazil)], E-mail: enio@vdg.fis.puc-rio.br

    2007-03-15

    Planetary magnetospheres, in which outer planet satellites orbit, are bombarded by energetic particles inducing chemical and physical changes in their icy surfaces. The existing condensed gases react to form new products, which then undergo thermal evolution from the natural day/night cycles of these satellites. Plasma irradiation of ice causes phase changes, e.g., water ice from crystalline to amorphous over short timescales. When ice is recrystallized by heating, the surface layers retain some disorder, which promote reactions among adsorbed molecules such as H{sub 2}O, CO{sub 2}, CH{sub 2}CO, HCOOH and theirs radiolysis products. In this work, chemical reactions involving formic acid condensed at 56 K are analyzed by using Plasma Desorption Mass Spectrometry-time-of-flight ({sup 252}Cf-PDMS-TOF). Mass spectra of positive and negative desorbed ions were obtained, giving information on the structure and abundance of the molecules on the ice; the expected cations and anions generated by the HCOOH dissociation have been observed. Furthermore, several series of cluster ions were also detected, all exhibiting the structure X{sub n}Y{sub m}R{sup {+-}}, where X and Y are the neutral ice molecules, such as HCOOH or H{sub 2}O, and R{sup {+-}} is either an atomic or a molecular ion, such as H{sup +}, H{sub 3}O{sup +} or COOH{sup -}. In general, the desorption yields of the observed positive and negative ions are characterized by a decreasing exponential function as the emitted ion mass increases; however, the (HCOOH){sub n}OH{sup -} series presents its maximum at n = 8.

  8. Matrix effects in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xiaoshan [Iowa State Univ., Ames, IA (United States)

    1995-07-07

    The inductively coupled plasma is an electrodeless discharge in a gas (usually Ar) at atmospheric pressure. Radio frequency energy generated by a RF power source is inductively coupled to the plasma gas through a water cooled load coil. In ICP-MS the "Fassel" TAX quartz torch commonly used in emission is mounted horizontally. The sample aerosol is introduced into the central flow, where the gas kinetic temperature is about 5000 K. The aerosol is vaporized, atomized, excited and ionized in the plasma, and the ions are subsequently extracted through two metal apertures (sampler and skimmer) into the mass spectrometer. In ICP-MS, the matrix effects, or non-spectroscopic interferences, can be defined as the type of interferences caused by dissolved concomitant salt ions in the solution. Matrix effects can be divided into two categories: (1) signal drift due to the deposition of solids on the sampling apertures; and/or (2) signal suppression or enhancement by the presence of the dissolved salts. The first category is now reasonably understood. The dissolved salts, especially refractory oxides, tend to deposit on the cool tip of the sampling cone. The clogging of the orifices reduces the ion flow into the ICP-MS, lowers the pressure in the first stage of ICP-MS, and enhances the level of metal oxide ions. Because the extent of the clogging increases with the time, the signal drifts down. Even at the very early stage of the development of ICP-MS, matrix effects had been observed. Houk et al. found out that the ICP-MS was not tolerant to solutions containing significant amounts of dissolved solids.

  9. Techniques for mass resolution improvement achieved by typical plasma mass analyzers: Modeling and simulations

    Science.gov (United States)

    Nicolaou, Georgios; Yamauchi, Masatoshi; Wieser, Martin; Barabash, Stas; Fedorov, Andrei

    2016-04-01

    Mass separation and particularly distinction between atomic ions and molecular ions are essential in understanding a wide range of plasma environments, with each consisted of different species with various properties. In this study we present the optimization results of light-weight (about 2 kg) magnetic mass analyzers with high g-factor for Rosetta (Ion Composition Analyser: ICA) and for Mars Express and Venus Express (Ion Mass Analyser: IMA). For the instrument's optimization we use SIMION, a 3D ion tracing software in which we can trace particle beams of several energies and directions, passing through the instrument's units. We first reproduced ICA and IMA results, which turned out to be different from simple models for low energy (< 100 eV). We then change the mechanical structure of several units of the instrument and we quantify the new mass resolution achieved with each change. Our goal is to find the optimal instrument's structure, which will allow us to achieve a proper mass resolution to distinguish atomic nitrogen from atomic oxygen for the purposes of a future magnetospheric mission.

  10. The plasma leptin concentration is closely associated with the body fat mass in nondiabetic uremic patients

    DEFF Research Database (Denmark)

    Clausen, P; Nielsen, P K; Olgaard, K

    1999-01-01

    Plasma leptin is associated with the body mass index and, more precisely, with the body fat mass. Plasma leptin has been found to be elevated in uremic patients. This study aimed at investigating the plasma leptin concentration and associations between plasma leptin, body fat mass, and glomerular...... filtration rate in nondiabetic predialysis uremic patients and in nondiabetic patients on chronic hemodialysis. Plasma leptin, body fat mass, and creatinine clearance were measured in 22 predialysis uremic patients, 18 hemodialysis patients, and 24 healthy control subjects. The logarithmically transformed...... plasma leptin concentration was closely associated with the body fat mass in all groups (r = 0.93, r = 0.83, and r = 0.72, respectively; p

  11. Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Baxter, Douglas C; Faarinen, Mikko; Österlund, Heléne; Rodushkin, Ilia; Christensen, Morten

    2011-09-01

    A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with (198)Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) μg L(-1) could be performed with uncertainty amplification factors levels of 0.14 μg L(-1), 0.35 μg L(-1) and 2.8 μg L(-1), with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

  12. Uranium quantification in semen by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Todorov, Todor I; Ejnik, John W; Guandalini, Gustavo; Xu, Hanna; Hoover, Dennis; Anderson, Larry; Squibb, Katherine; McDiarmid, Melissa A; Centeno, Jose A

    2013-01-01

    In this study we report uranium analysis for human semen samples. Uranium quantification was performed by inductively coupled plasma mass spectrometry. No additives, such as chymotrypsin or bovine serum albumin, were used for semen liquefaction, as they showed significant uranium content. For method validation we spiked 2g aliquots of pooled control semen at three different levels of uranium: low at 5 pg/g, medium at 50 pg/g, and high at 1000 pg/g. The detection limit was determined to be 0.8 pg/g uranium in human semen. The data reproduced within 1.4-7% RSD and spike recoveries were 97-100%. The uranium level of the unspiked, pooled control semen was 2.9 pg/g of semen (n=10). In addition six semen samples from a cohort of Veterans exposed to depleted uranium (DU) in the 1991 Gulf War were analyzed with no knowledge of their exposure history. Uranium levels in the Veterans' semen samples ranged from undetectable (<0.8 pg/g) to 3350 pg/g. This wide concentration range for uranium in semen is consistent with known differences in current DU body burdens in these individuals, some of whom have retained embedded DU fragments.

  13. Uranium quantification in semen by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Todorov, Todor; Ejnik, John W.; Guandalini, Gustavo S.; Xu, Hanna; Hoover, Dennis; Anderson, Larry W.; Squibb, Katherine; McDiarmid, Melissa A.; Centeno, Jose A.

    2013-01-01

    In this study we report uranium analysis for human semen samples. Uranium quantification was performed by inductively coupled plasma mass spectrometry. No additives, such as chymotrypsin or bovine serum albumin, were used for semen liquefaction, as they showed significant uranium content. For method validation we spiked 2 g aliquots of pooled control semen at three different levels of uranium: low at 5 pg/g, medium at 50 pg/g, and high at 1000 pg/g. The detection limit was determined to be 0.8 pg/g uranium in human semen. The data reproduced within 1.4–7% RSD and spike recoveries were 97–100%. The uranium level of the unspiked, pooled control semen was 2.9 pg/g of semen (n = 10). In addition six semen samples from a cohort of Veterans exposed to depleted uranium (DU) in the 1991 Gulf War were analyzed with no knowledge of their exposure history. Uranium levels in the Veterans’ semen samples ranged from undetectable (<0.8 pg/g) to 3350 pg/g. This wide concentration range for uranium in semen is consistent with known differences in current DU body burdens in these individuals, some of whom have retained embedded DU fragments.

  14. Mass and energy of erupting solar plasma observed with the X-Ray Telescope on Hinode

    CERN Document Server

    Lee, Jin-Yi; Reeves, Katharine K; Moon, Yong-Jae; Kim, Kap-Sung

    2014-01-01

    We investigate seven eruptive plasma observations by Hinode/XRT. Their corresponding EUV and/or white light CME features are visible in some events. Five events are observed in several passbands in X-rays, which allows the determination of the eruptive plasma temperature using a filter ratio method. We find that the isothermal temperatures vary from 1.6 to 10 MK. These temperatures are an average weighted toward higher temperature plasma. We determine the mass constraints of eruptive plasmas by assuming simplified geometrical structures of the plasma with isothermal plasma temperatures. This method provides an upper limit to the masses of the observed eruptive plasmas in X-ray passbands since any clumping causes the overestimation of the mass. For the other two events, we assume the temperatures are at the maximum temperature of the XRT temperature response function, which gives a lower limit of the masses. We find that the masses in XRT, ~3x10 13 - 5x10 14 g, are smaller in their upper limit than total masse...

  15. Damping of electron center-of-mass oscillation in ultracold plasmas

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Wei-Ting; Witte, Craig; Roberts, Jacob L. [Department of Physics, Colorado State University, Fort Collins, Colorado 80523 (United States)

    2016-05-15

    Applying a short electric field pulse to an ultracold plasma induces an electron plasma oscillation. This manifests itself as an oscillation of the electron center of mass around the ion center of mass in the ultracold plasma. In general, the oscillation can damp due to either collisionless or collisional mechanisms, or a combination of the both. To investigate the nature of oscillation damping in ultracold plasmas, we developed a molecular dynamics model of the ultracold plasma electrons. Through this model, we found that depending on the neutrality of the ultracold plasma and the size of an applied DC electric field, there are some parameter ranges where the damping is primarily collisional and some primarily collisionless. We conducted experiments to compare the measured damping rate with theory predictions and found them to be in good agreement. Extension of our measurements to different parameter ranges should enable studies for strong-coupling influence on electron-ion collision rates.

  16. New Applications of Inductively Coupled Plasma-Mass Spectrometry in the Nuclear Industry

    Energy Technology Data Exchange (ETDEWEB)

    Rob Henry; Dagmar Koller; Phil Marriott

    1998-12-31

    Inductively coupled plasma mass spectrometry (ICP-MS) complements the traditional methods of quantitation of radioactive isotopes. Because of the favorable ionization potential of most actinides and their daughter products, the argon plasma provides a rich, stable source of ions, which are introduced through a plasma-mass spectrometer interface into the mass spectrometer for isotopic separation. Samples are normally introduced in solution, although direct solids analysis has also been achieved using laser ablation of the sample into the argon plasma. Since 1983, improvements in ICP-MS sensitivity have resulted in correspondingly lower mass detection capability. This development has in turn expanded the number of isotopes accessible to measurement at the levels required in the nuclear industry.

  17. MASS AND ENERGY OF ERUPTING SOLAR PLASMA OBSERVED WITH THE X-RAY TELESCOPE ON HINODE

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jin-Yi; Moon, Yong-Jae; Kim, Kap-Sung [Department of Astronomy and Space Science, Kyung Hee University, Yongin, Gyeonggi 446-701 (Korea, Republic of); Raymond, John C.; Reeves, Katharine K., E-mail: jlee@khu.ac.kr [Harvard-Smithsonian Center for Astrophysics, Cambridge, MA 02138 (United States)

    2015-01-10

    We investigate seven eruptive plasma observations by Hinode/XRT. Their corresponding EUV and/or white light coronal mass ejection features are visible in some events. Five events are observed in several passbands in X-rays, which allows for the determination of the eruptive plasma temperature using a filter ratio method. We find that the isothermal temperatures vary from 1.6 to 10 MK. These temperatures are an average weighted toward higher temperature plasma. We determine the mass constraints of eruptive plasmas by assuming simplified geometrical structures of the plasma with isothermal plasma temperatures. This method provides an upper limit to the masses of the observed eruptive plasmas in X-ray passbands since any clumping causes the overestimation of the mass. For the other two events, we assume the temperatures are at the maximum temperature of the X-ray Telescope (XRT) temperature response function, which gives a lower limit of the masses. We find that the masses in XRT, ∼3 × 10{sup 13}-5 × 10{sup 14} g, are smaller in their upper limit than the total masses obtained by LASCO, ∼1 × 10{sup 15} g. In addition, we estimate the radiative loss, thermal conduction, thermal, and kinetic energies of the eruptive plasma in X-rays. For four events, we find that the thermal conduction timescales are much shorter than the duration of eruption. This result implies that additional heating during the eruption may be required to explain the plasma observations in X-rays for the four events.

  18. Intermediate mass dilepton production during the chemical equilibration of quark gluon plasma

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The production of dileptons from the chemically equilibrating quark gluon plasma in the intermediate mass region has been studied. Comparing with the calculated results based on the thermodynamic equilibrium system of quark gluon plasma, it has been found that the quark phase of the chemically equilibrating system gives rise to an even larger enhancement of the dileptons production. Therefore, such an enhancement of dilepton production may signal the formation of quark gluon plasma.

  19. Determination of selenoprotein P in human plasma by solid phase extraction and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Bendahl, L.; Sidenius, U.; Gammelgaard, Bente

    2000-01-01

    measured by inductively coupled plasma mass spectrometry (ICP-MS) monitoring the Se-82 isotope. Linear response was observed in the concentration range 0.3-70.8 mu g/l selenium as selenoprotein P with a correlation coefficient of 0.9994. The precision expressed as relative standard deviation was better...

  20. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-01-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  1. Solvent extraction, ion chromatography, and mass spectrometry of molybdenum isotopes.

    Science.gov (United States)

    Dauphas, N; Reisberg, L; Marty, B

    2001-06-01

    A procedure was developed that allows precise determination of molybdenum isotope abundances in natural samples. Purification of molybdenum was first achieved by solvent extraction using di(2-ethylhexyl) phosphate. Further separation of molybdenum from isobar nuclides was obtained by ion chromatography using AG1-X8 strongly basic anion exchanger. Finally, molybdenum isotopic composition was measured using a multiple collector inductively coupled plasma hexapole mass spectrometer. The abundances of molybdenum isotopes 92, 94, 95, 96, 97, 98, and 100 are 14.8428(510), 9.2498(157), 15.9303(133), 16.6787(37), 9.5534(83), 24.1346(394), and 9.6104(312) respectively, resulting in an atomic mass of 95.9304(45). After internal normalization for mass fractionation, no variation of the molybdenum isotopic composition is observed among terrestrial samples within a relative precision on the order of 0.00001-0.0001. This demonstrates the reliability of the method, which can be applied to searching for possible isotopic anomalies and mass fractionation.

  2. Plasma-based ambient mass spectrometry techniques: The current status and future prospective.

    Science.gov (United States)

    Ding, Xuelu; Duan, Yixiang

    2015-01-01

    Plasma-based ambient mass spectrometry is emerging as a frontier technology for direct analysis of sample that employs low-energy plasma as the ionization reagent. The versatile sources of ambient mass spectrometry (MS) can be classified according to the plasma formation approaches; namely, corona discharge, glow discharge, dielectric barrier discharge, and microwave-induced discharge. These techniques allow pretreatment-free detection of samples, ranging from biological materials (e.g., flies, bacteria, plants, tissues, peptides, metabolites, and lipids) to pharmaceuticals, food-stuffs, polymers, chemical warfare reagents, and daily-use chemicals. In most cases, plasma-based ambient MS performs well as a qualitative tool and as an analyzer for semi-quantitation. Herein, we provide an overview of the key concepts, mechanisms, and applications of plasma-based ambient MS techniques, and discuss the challenges and outlook.

  3. Mass spectroscopy of the ion flux produced during inductively coupled plasma nitriding process

    Science.gov (United States)

    Kolodko, D. V.; Kaziev, A. V.; Ageychenkov, D. G.; Meshcheryakova, E. A.; Pisarev, A. A.; Tumarkin, A. V.

    2017-05-01

    Ion fluxes on the surface of sample embedded in inductively coupled plasma have been studied in conditions typical for titanium alloy nitriding: total pressure 0.44 Pa, Ar/N2 = 70%/30%, and RF power 1500 W. The gas composition was independently monitored by the quadrupole analyser. The ion fluxes were sampled using a specially designed electrostatic extractor and then analysed with a magnetic sector mass-separator. The extractor design allowed us to apply a bias voltage to the plasma facing electrode thus imitating interaction of ions with the surface during the plasma processing. The ion fluxes of Ar+, {{{N}}}2{}+, and N+ on the surface were measured. The mass spectroscopy diagnostics unit is suitable for extensive ion content studies in the plasma technology facilities.

  4. Proteomic biomarker discovery in 1000 human plasma samples with mass spectrometry

    DEFF Research Database (Denmark)

    Cominetti, Ornella; Núñez Galindo, Antonio; Corthésy, John

    2016-01-01

    the quality of the MS data and provided descriptive statistics. The data set was interrogated for proteins with most stable expression levels in that set of plasma samples. We evaluated standard clinical variables that typically impact forthcoming results and assessed body mass index-associated and gender......-specific proteins at two time points. We demonstrate that analyzing a large number of human plasma samples for biomarker discovery with MS using isobaric tagging is feasible, providing robust and consistent biological results....

  5. Diagnostics of low and atmospheric pressure plasmas by means of mass spectrometry

    CERN Document Server

    Benedikt, Jan; von Keudell, Achim

    2011-01-01

    The knowledge of absolute fluxes of reactive species such as radicals or energetic ions to the surface is crucial for understanding the growth or etching of thin films. These species have due to their high reactivity very low densities and their detection is therefore a challenging task. Mass spectrometry is a very sensitive technique and it will be demonstrated that it is a good choice for the study of plasma chemistry. Mass spectrometry measures the plasma composition directly at the surface and is not limited by existence of accessible optical transitions. When properly designed and carefully calibrated mass spectrometry provides absolute densities of the measured species. It can even measure internally excited metastable species. Here, measurement of neutral species and positive ions generated in an atmospheric pressure plasmas jet operated with He, hexamethyldisiloxane and O2 will be presented.

  6. Direct analysis of samples by mass spectrometry: From elements to bio-molecules using laser ablation inductively couple plasma mass spectrometry and laser desorption/ionization mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Perdian, David C. [Iowa State Univ., Ames, IA (United States)

    2009-01-01

    Mass spectrometric methods that are able to analyze solid samples or biological materials with little or no sample preparation are invaluable to science as well as society. Fundamental research that has discovered experimental and instrumental parameters that inhibit fractionation effects that occur during the quantification of elemental species in solid samples by laser ablation inductively coupled plasma mass spectrometry is described. Research that determines the effectiveness of novel laser desorption/ionization mass spectrometric methods for the molecular analysis of biological tissues at atmospheric pressure and at high spatial resolution is also described. A spatial resolution is achieved that is able to analyze samples at the single cell level.

  7. Electrospray ionization Fourier transform mass spectrometric analysis of intact bikunin glycosaminoglycan from normal human plasma.

    Science.gov (United States)

    Laremore, Tatiana N; Leach, Franklin E; Amster, I Jonathan; Linhardt, Robert J

    2011-08-15

    A mixture of glycosaminoglycan (GAG) chains from a plasma proteoglycan bikunin was fractionated using native, continuous-elution polyacrylamide gel electrophoresis, and the resulting fractions were analyzed by electrospray ionization Fourier transform mass spectrometry (ESI FTMS). Molecular mass analysis of the intact GAG afforded information about the length and composition of GAG chains in the mixture. Ambiguity in the interpretation of the intact GAG mass spectra was eliminated by conducting an additional experiment in which the GAG chains of known molecular mass were treated with a GAG-degrading enzyme, chondroitinase ABC, and the digestion products were analyzed by ESI FTMS. The plasma bikunin GAG chains consisted predominantly of odd number of saccharides, although few chains consisting of even number of saccharides were also detected. Majority of the analyzed chains were tetrasulfated or pentasulfated and comprised by 29 to 41 monosaccharides.

  8. An argon–nitrogen–hydrogen mixed-gas plasma as a robust ionization source for inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Makonnen, Yoseif; Beauchemin, Diane, E-mail: diane.beauchemin@chem.queensu.ca

    2014-09-01

    Multivariate optimization of an argon–nitrogen–hydrogen mixed-gas plasma for minimum matrix effects, while maintaining analyte sensitivity as much as possible, was carried out in inductively coupled plasma mass spectrometry. In the presence of 0.1 M Na, the 33.9 ± 3.9% (n = 13 elements) analyte signal suppression on average observed in an all-argon plasma was alleviated with the optimized mixed-gas plasma, the average being − 4.0 ± 8.8%, with enhancement in several cases. An addition of 2.3% v/v N{sub 2} in the outer plasma gas, and 0.50% v/v H{sub 2} to the central channel, as a sheath around the nebulizer gas flow, was sufficient for this drastic increase in robustness. It also reduced the background from ArO{sup +} and Ar{sub 2}{sup +} as well as oxide levels by over an order of magnitude. On the other hand, the background from NO{sup +} and ArN{sup +} increased by up to an order of magnitude while the levels of doubly-charged ions increased to 7% (versus 2.7% in an argon plasma optimized for sensitivity). Furthermore, detection limits were generally degraded by 5 to 15 fold when using the mixed-gas plasma versus the argon plasma for matrix-free solution (although they were better for several elements in 0.1 M Na). Nonetheless, the drastically increased robustness allowed the direct quantitative multielement analysis of certified ore reference materials, as well as the determination of Mo and Cd in seawater, without using any matrix-matching or internal standardization. - Highlights: • Addition of N{sub 2} to the plasma gas and H{sub 2} as a sheath gas results in a very robust ICP. • ArO{sup +} and Ar{sub 2}{sup +} background and oxide levels are reduced by over an order of magnitude. • Multielement analysis of rock digests is possible with a simple external calibration. • No internal standardization or matrix-matching is required for accurate analysis. • Cd and Mo were accurately determined in undiluted seawater.

  9. The effects of analyte mass and collision gases on ion beam formation in an inductively coupled plasma mass spectrometer

    Science.gov (United States)

    Larsen, Jessica J.; Edmund, Alisa J.; Farnsworth, Paul B.

    2016-11-01

    Planar laser induced fluorescence (PLIF) was used to evaluate the effect of matrix components on the formation and focusing of a Ba ion beam in a commercial inductively coupled plasma mass spectrometer. Cross sections of the ion beams were taken in the second vacuum stage, in front of the entrance to the mass analyzer. Under normal operating conditions, the addition of Pb shifted the position of the Ba ion beam to the right. PLIF was also used to evaluate the effect of a collision reaction interface (CRI) on Ca and Ba ion beams. A wider velocity distribution of ions and a decrease in overall intensity were observed for the CRI images. The fluorescence and mass spectrometer signals decreased with increased CRI flow rates. These effects were most obvious for Ca ions with He gas.

  10. Lifetime Calculations on Collector Optics from Laser Plasma Extreme Ultraviolet Sources with Minimum Mass

    Institute of Scientific and Technical Information of China (English)

    WU Tao; WANG Xin-Bing

    2011-01-01

    An ion flux and its kinetic energy spectrum are obtained using a self similar spherically symmetric fluid model of expansion of a collisionless plasma into vacuum. According to the ion flux and energy distribution, the collector optical lifetime is estimated by knowledge of the sputtering yield of conventional Mo/Si multilayer coatings for the CO2 and Nd:YAG pulsed-laser produced plasmas based on the minimum mass tin droplet target without debris mitigation. The results show that the longer wavelength of the CO2 laser produced plasma light source is more suitable for extreme ultraviolet lithography than Nd:YAG laser in respect of fast ion debris induced sputtering damage to the collector mirror.%@@ An ion flux and its kinetic energy spectrum are obtained using a self similar spherically symmetric fluid model of expansion of a collisionless plasma into vacuum.According to the ion flux and energy distribution,the collector optical lifetime is estimated by knowledge of the sputtering yield of conventional Mo/Si multilayer coatings for the CO2 and Nd:YAG pulsed-laser produced plasmas based on the minimum mass tin droplet target without debris mitigation.The results show that the longer wavelength of the CO2 laser produced plasma light source is more suitable for extreme ultraviolet lithography than Nd:YAG laser in respect of fast ion debris induced sputtering damage to the collector mirror.

  11. Determination of Arsenic in Sinus Wash and Tap Water by Inductively Coupled Plasma-Mass Spectrometry

    Science.gov (United States)

    Donnell, Anna M.; Nahan, Keaton; Holloway, Dawone; Vonderheide, Anne P.

    2016-01-01

    Arsenic is a toxic element to which humans are primarily exposed through food and water; it occurs as a result of human activities and naturally from the earth's crust. An experiment was developed for a senior level analytical laboratory utilizing an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) for the analysis of arsenic in household…

  12. Independent prognostic value of left ventricular mass, diastolic function, and fasting plasma glucose

    DEFF Research Database (Denmark)

    Pareek, Manan; Nielsen, Mette Lundgren; Leósdóttir, Margrét

    2016-01-01

    OBJECTIVE: To explore the independent prognostic value of left ventricular (LV) mass, diastolic function, and fasting plasma glucose (FPG) for the prediction of incident cardiac events in a random population sample. DESIGN AND METHOD: 415 women and 999 men aged 56-79 years, included between 2002...

  13. Determination of platinum in human subcellular microsamples by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Björn, Erik; Nygren, Yvonne; Nguyen, Tam T. T. N.

    2007-01-01

    A fast and robust method for the determination of platinum in human subcellular microsamples by inductively coupled plasma mass spectrometry was developed, characterized, and validated. Samples of isolated DNA and exosome fractions from human ovarian (2008) and melanoma (T289) cancer cell lines...

  14. Mass identification of the neutral products generated in the plasma treatment of polluted atmospheres

    Science.gov (United States)

    Seymour, David

    2013-09-01

    Plasmas produced using Dielectric Barrier Discharge (DBD) devices are very effective in the abatement of air pollution resulting from, for example, the emission of volatile organic compounds (VCOs) by a range of industrial and agricultural processes. The development and monitoring of effective DBD systems can be investigated by advanced mass spectrometric methods specifically configured for analysis at high and atmospheric pressures The present work involves the operation of a small DBD reactor which uses either a helium or nitrogen carrier gas to sustain the plasma to which may be added reactive gases, such as oxygen, as well as samples of pollutants such as chlorinated hydrocarbons, including trichloroethylene. The mass spectrometric analysis was performed using a specially configured system manufactured by Hiden Analytical Ltd. The DBD source may also be combined with a catalyst for plasma-enhanced catalysis. The neutral products of the reactions proceeding in the plasma at atmospheric pressure are sampled through the capillary sampling system which also reduces the pressure of the gas mixture delivered to the ionisation source of the quadrupole mass spectrometer. The ions produced are subsequently mass identified. We describe typical data and comment on the advantages of this technique.

  15. Determination of albendazole sulfoxide in human plasma by using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Saraner, Nihal; Özkan, Güler Yağmur; Güney, Berrak; Alkan, Erkin; Burul-Bozkurt, Nihan; Sağlam, Onursal; Fikirdeşici, Ezgi; Yıldırım, Mevlüt

    2016-06-01

    A rapid, simple and sensitive method was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determination of albendazole sulfoxide (ABZOX) in human plasma. The plasma samples were extracted by protein precipitation using albendazole sulfoxide-d3 as internal standard (IS). The chromatographic separation was performed on Waters Xbridge C18Column (100×4.6mm, 3.5μm) with a mobile phase consisting of ammonia solution, water and methanol at a flow rate of 0.70mL/min. ABZOX was detected and identified by mass spectrometry with electrospray ionization (ESI) in positive ion and multiple-reaction monitoring (MRM) mode. The method was linear in the range of 3-1500ng/mL for ABZOX. This method was successfully applied to the bioequivalence study in human plasma samples.

  16. Fundamental studies of the plasma extraction and ion beam formation processes in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Niu, Hongsen

    1995-02-10

    The fundamental and practical aspects are described for extracting ions from atmospheric pressure plasma sources into an analytical mass spectrometer. Methodologies and basic concepts of inductively coupled plasma mass spectrometry (ICP-MS) are emphasized in the discussion, including ion source, sampling interface, supersonic expansion, slumming process, ion optics and beam focusing, and vacuum considerations. Some new developments and innovative designs are introduced. The plasma extraction process in ICP-MS was investigated by Langmuir measurements in the region between the skimmer and first ion lens. Electron temperature (T{sub e}) is in the range 2000--11000 K and changes with probe position inside an aerosol gas flow. Electron density (n{sub e}) is in the range 10{sup 8}--10{sup 10} {sup {minus}cm }at the skimmer tip and drops abruptly to 10{sup 6}--10{sup 8} cm{sup {minus}3} near the skimmer tip and drops abruptly to 10{sup 6}--10{sup 8} cm{sup {minus}3} downstream further behind the skimmer. Electron density in the beam leaving the skimmer also depends on water loading and on the presence and mass of matrix elements. Axially resolved distributions of electron number-density and electron temperature were obtained to characterize the ion beam at a variety of plasma operating conditions. The electron density dropped by a factor of 101 along the centerline between the sampler and skimmer cones in the first stage and continued to drop by factors of 10{sup 4}--10{sup 5} downstream of skimmer to the entrance of ion lens. The electron density in the beam expansion behind sampler cone exhibited a 1/z{sup 2} intensity fall-off (z is the axial position). An second beam expansion originated from the skimmer entrance, and the beam flow underwent with another 1/z{sup 2} fall-off behind the skimmer. Skimmer interactions play an important role in plasma extraction in the ICP-MS instrument.

  17. Inductively coupled plasma mass spectrometry in the analysis of biological samples and pharmaceutical drugs

    Science.gov (United States)

    Ossipov, K.; Seregina, I. F.; Bolshov, M. A.

    2016-04-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in the analysis of biological samples (whole blood, serum, blood plasma, urine, tissues, etc.) and pharmaceutical drugs. The shortcomings of this method related to spectral and non-spectral interferences are manifested in full measure in determination of the target analytes in these complex samples strongly differing in composition. The spectral interferences are caused by similarity of masses of the target component and sample matrix components. Non-spectral interferences are related to the influence of sample matrix components on the physicochemical processes taking place during formation and transportation of liquid sample aerosols into the plasma, on the value and spatial distribution of plasma temperature and on the transmission of the ion beam from the interface to mass spectrometer detector. The review is devoted to analysis of different mechanisms of appearance of non-spectral interferences and to ways for their minimization or elimination. Special attention is paid to the techniques of biological sample preparation, which largely determine the mechanisms of the influence of sample composition on the results of element determination. The ways of lowering non-spectral interferences by instrumental parameter tuning and application of internal standards are considered. The bibliography includes 189 references.

  18. Liquid chromatography-mass spectrometric determination of rufinamide in low volume plasma samples.

    Science.gov (United States)

    Gáll, Zsolt; Vancea, Szende; Dogaru, Maria T; Szilágyi, Tibor

    2013-12-01

    Quantification of rufinamide in plasma was achieved using a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method. The chromatographic separation was achieved on a reversed phase column (Zorbax SB-C18 100mm×3mm, 3.5μm) under isocratic conditions. The mobile phase consisted of a mixture of water containing 0.1% formic acid and methanol (50:50, v/v). The mass spectrometric detection of the analyte was in multiple reaction monitoring mode (MRM) using an electrospray positive ionization (ESI positive). The monitored ions were 127m/z derived from 239m/z rufinamide and 108m/z derived from 251m/z the internal standard (lacosamide). Protein precipitation with methanol was applied for sample preparation using only 50μl aliquots. The concentration range was 40-2000ng/ml for rufinamide in plasma. The limit of detection was 1.25ng/ml and the lower limit of quantification was established at 5ng/ml rufinamide concentration. Selectivity and matrix effect was verified using individual human, rat and rabbit plasma samples. Short-term, post-preparative and freeze-thaw stability was also investigated. The proposed method provides accuracy, precision and high-throughput (short runtime 4.5min) for quantitative determination of rufinamide in plasma. This is the first reported liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for analysis of rufinamide from low volume plasma samples. The LC-MS/MS method was validated according to the current official guidelines and can be applied to accurately measure rufinamide level of large number of plasma samples from clinical studies or therapeutic drug monitoring.

  19. Inductively coupled plasma mass spectrometry for stable isotope metabolic tracer studies of living systems

    Energy Technology Data Exchange (ETDEWEB)

    Luong, Elise [Iowa State Univ., Ames, IA (United States)

    1999-05-10

    This dissertation focuses on the development of methods for stable isotope metabolic tracer studies in living systems using inductively coupled plasma single and dual quadrupole mass spectrometers. Sub-nanogram per gram levels of molybdenum (Mo) from human blood plasma are isolated by the use of anion exchange alumina microcolumns. Million-fold more concentrated spectral and matrix interferences such as sodium, chloride, sulfate, phosphate, etc. in the blood constituents are removed from the analyte. The recovery of Mo from the alumina column is 82 ± 5% (n = 5). Isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is utilized for the quantitative ultra-trace concentration determination of Mo in bovine and human blood samples. The average Mo concentration in reference bovine serum determined by this method is 10.2 ± 0.4 ng/g, while the certified value is 11.5 ± 1.1 ng/g (95% confidence interval). The Mo concentration of one pool of human blood plasma from two healthy male donors is 0.5 ± 0.1 ng/g. The inductively coupled plasma twin quadrupole mass spectrometer (ICP-TQMS) is used to measure the carbon isotope ratio from non-volatile organic compounds and bio-organic molecules to assess the ability as an alternative analytical method to gas chromatography combustion isotope ratio mass spectrometry (GC-combustion-IRMS). Trytophan, myoglobin, and β-cyclodextrin are chosen for the study, initial observation of spectral interference of 13C+ with 12C 1H+ comes from the incomplete dissociation of myoglobin and/or β-cyclodextrin.

  20. Measurement of the 135Cs half-life with accelerator mass spectrometry and inductively coupled plasma mass spectrometry

    Science.gov (United States)

    MacDonald, C. M.; Cornett, R. J.; Charles, C. R. J.; Zhao, X. L.; Kieser, W. E.

    2016-01-01

    The isotope 135Cs is quoted as having a half-life of 2.3 Myr. However, there are three published values ranging from 1.8 to 3 Myr. This research reviews previous measurements and reports a new measurement of the half-life using newly developed accelerator mass spectrometry (AMS) and inductively coupled plasma mass spectrometry (ICPMS) techniques along with β and γ radiometric analysis. The half-life was determined to be (1.6 ±0.6 ) ×106 yr by AMS and (1.3 ±0.2 ) ×106 yr by ICPMS with 95% confidence. The two values agree with each other but differ from the accepted value by ˜40 % .

  1. Identification of phosphorylated butyrylcholinesterase in human plasma using immunoaffinity purification and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Aryal, Uma K.; Lin, Chiann Tso; Kim, Jong Seo; Heibeck, Tyler H.; Wang, Jun; Qian, Weijun; Lin, Yuehe

    2012-04-20

    Paraoxon (diethyl 4-nitrophenyl phosphate) is an active metabolite of the common insecticide parathion and is acutely toxic due to the inhibition of cholinesterase (ChE) activity in the nervous systems. The Inhibition of butyrylcholinesterase (BChE) activity by paraoxon is due to the formation of phosphorylated BChE adduct, and the detection of the phosphorylated BChE adduct in human plasma can serve as an exposure biomarker of organophosphate pesticides and nerve agents. In this study, we performed immunoaffinity purification and liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis for identifying phosphorylated BChE in human plasma treated by paraoxon. BChE was captured by biotinylated anti-BChE polyclonal antibodies conjugated to streptavidin magnetic beads. Western blot analysis showed that the antibody was effective to recognize both native and modified BChE with high specificity. The exact phosphorylation site of BChE was confirmed on Serine 198 by MS/MS with a 108 Da modification mass and accurately measured parent ion masses. The phosphorylated BChE peptide was also successfully detected in the immunoaffinity purified sample from paraoxon treated human plasma. Thus, immunoaffinity purification combined with mass spectrometry represents a viable approach for the detection of paraoxon-modified BChE and other forms of modified BChE as exposure biomarkers of organophosphates and nerve agents.

  2. Characterization of the seminal plasma proteome in men with prostatitis by mass spectrometry

    Directory of Open Access Journals (Sweden)

    Kagedan Daniel

    2012-02-01

    Full Text Available Abstract Background Prostatitis is an inflammation of the prostate gland which affects approximately 10% of men. Despite its frequency, diagnosing prostatitis and monitoring patient response to treatment remains frustrating. As the prostate contributes a substantial percentage of proteins to seminal plasma, we hypothesized that a protein biomarker of prostatitis might be found by comparing the seminal plasma proteome of patients with and without prostatitis. Results Using mass spectrometry, we identified 1708 proteins in the pooled seminal plasma of 5 prostatitis patients. Comparing this list to a previously published list of seminal plasma proteins in the pooled seminal plasma of 5 healthy, fertile controls yielded 1464 proteins in common, 413 found only in the control group, and 254 found only in the prostatitis group. Applying a set of criteria to this dataset, we generated a high-confidence list of 59 candidate prostatitis biomarkers, 33 of which were significantly increased in prostatitis as compared to control, and 26 of which were decreased. The candidates were analyzed using Gene Ontology and Ingenuity Pathway analysis to delineate their subcellular localizations and functions. Conclusions Thus, in this study, we identified 59 putative biomarkers in seminal plasma that need further validation for diagnosis and monitoring of prostatitis.

  3. The effect of plasma operating parameters on analyte signals in inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Horlick, G.; Tan, S. H.; Vaughan, M. A.; Rose, C. A.

    Utilizing the SCIEX ICP-MS an extensive study of the effects that plasma operating parameters have on analyte ion signals in ICP-MS has been carried out. Parameters studied included aerosol flow rate (nebulizer pressure), auxiliary flow rate, power and sampling depth (sampling position from the load coil). The two key parameters are aerosol flow rate (nebulizer pressure) and power. Elements can be grouped into characteristic behaviour patterns based on the overall dependence of their ion count signal on these two parameters. The nebulizer pressure-power behavior patterns allow a sensible selection of compromise operating conditions and significantly clarify single parameter observations which often indicate confusing trends in behavior. In addition to characterizing analyte ion signals the parameter behavior plots have also been used to study oxide species and plus two ions in ICP-MS. While aerosol flow rate and power appear to be the key ICP parameters in ICP-MS, ion signals are dependent on sampling depth and auxiliary flow rate and some data are also presented illustrating the signal dependence on these two parameters.

  4. Determination of loperamide in human plasma and saliva by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Arafat, Tawfiq; Arafat, Basil; awad, Riad; awwad, Ahmad Abu

    2014-12-01

    A simple and sensitive liquid chromatography-tandem mass spectrometric method for quantification of loperamide in human plasma and saliva was developed and validated, and then successfully applied in pharmacokinetic clinical study to investigate and correlate bioavailability of Imodium(®) 2mg quartet tablet dose in both human plasma and saliva. Loperamide with labeled internal standard was extracted from its biological matrix by methanol as protein direct precipitant in single extraction step. Adequate chromatographic separation for analytes from plasma and saliva matrices was achieved using ACE C18 (50mm×2.1mm, 5μm) column, eluted by water/methanol/formic acid (30:70:0.1%, v/v), delivered isocratically at constant flow rate of 0.75ml/min. The method validation intends to investigate specificity, sensitivity, linearity, precision, accuracy, recovery, matrix effect and stability according to European guideline, and partial validation was applied on saliva, specificity, matrix effect, recovery, sensitivity, within and between day precision and accuracy. The calibration curve was linear through the range of 20-3000pg/ml in both plasma and saliva using a 50μl sample volume. The partial validation sections outcome in saliva was so close to those in plasma. The within- and between-day precisions were all below 8.7% for plasma and below 11.4% for saliva. Accuracies ranged from 94 to 105% for both matrices. In this study, 26 healthy volunteers participated in the clinical study, and 6 of gave their saliva samples in addition to plasma at the same time schedule. The pharmacokinetic parameters of Cmax, AUC0-t and AUC0-∞, Tmax and T1/2 in both plasma and saliva were calculated and correlated.

  5. Multimycotoxin analysis in water and fish plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Tolosa, J; Font, G; Mañes, J; Ferrer, E

    2016-02-01

    High performance liquid chromatography-mass spectrometry was used for the determination of 15 mycotoxins in water and fish plasma samples, including aflatoxins, fumonisins, ochratoxin A, sterigmatocistin, fusarenon-X and emerging Fusarium mycotoxins. In this work, dispersive liquid-liquid microextraction (DLLME) was assessed as a sample treatment for the simultaneous extraction of mycotoxins. Results showed differences in recovery assays when different extraction solvents were employed. Ethyl acetate showed better recoveries for the major part of mycotoxins analyzed, except for aflatoxins B2, G1 and G2, which showed better recoveries when employing chloroform as extractant solvent. Fumonisins and beauvericin exhibited low recoveries in both water and plasma. This method was validated according to guidelines established by European Commission and has shown to be suitable to be applied in dietary and/or toxicokinetic studies in fish where is necessary to check mycotoxin contents in rearing water and fish plasma.

  6. Determination of carbocysteine in human plasma by liquid chromatography/tandem mass spectrometry employing precolumn derivatization.

    Science.gov (United States)

    Chen, Xiaoyan; Zhong, Dafang; Han, Ying; Xie, Zhiyong

    2003-01-01

    A sensitive liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was developed to determine carbocysteine in human plasma using 2-pyridylacetic acid as the internal standard (IS). The method employed derivatization with 10 M hydrochloric acid/methanol, which significantly improved the ionization efficiency of carbocysteine. After methanol-induced protein precipitation of plasma samples, carbocysteine and the IS were derivatized and subjected to LC/MS/MS analysis using atmospheric pressure chemical ionization. The method has a lower limit of quantitation of 20 ng/mL for a 0.2-mL plasma aliquot. The intra- and inter-day precision (RSD), calculated from quality control (QC) samples, was less than 7%. The accuracy, determined using QC samples, was within +/- 1%. The method offered increased sensitivity, selectivity and speed of analysis over existing methods. The method was utilized to support clinical pharmacokinetic studies of carbocysteine in volunteers following oral administration. Copyright 2002 John Wiley & Sons, Ltd.

  7. Standard practice for alternate actinide calibration for inductively coupled plasma-mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 This practice provides guidance for an alternate linear calibration for the determination of selected actinide isotopes in appropriately prepared aqueous solutions by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). This alternate calibration is mass bias adjusted using thorium-232 (232Th) and uranium-238 (238U) standards. One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities. Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest. 1.2 The instrument response for a series of determinations of known concentration of 232Th and 238U defines the mass versus response relationship. For each standard concentration, the slope of the line defined by 232Th and 238U is used to derive linear calibration curves for each mass of interest using interference equ...

  8. Effect of catecholamines and insulin on plasma volume and intravascular mass of albumin in man

    DEFF Research Database (Denmark)

    Hilsted, J; Christensen, N J; Larsen, S

    1989-01-01

    1. The effect of intravenous catecholamine infusions and of intravenous insulin on plasma volume and intravascular mass of albumin was investigated in healthy males. 2. Physiological doses of adrenaline (0.5 microgram/min and 3 microgram/min) increased peripheral venous packed cell volume...... significantly; intravenous noradrenaline at 0.5 microgram/min had no effect on packed cell volume, whereas packed cell volume increased significantly at 3 micrograms of noradrenaline/min. No significant change in packed cell volume was found during saline infusion. 3. During adrenaline infusion at 6 micrograms...... in packed cell volume, plasma volume, intravascular mass of albumin and transcapillary escape rate of albumin during hypoglycaemia may be explained by the combined actions of adrenaline and insulin....

  9. Thorium colloid analysis by single particle inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Degueldre, C; Favarger, P-Y

    2004-04-19

    Thorium colloid analysis in water has been carried out by a single particle mode using inductively coupled plasma mass spectrometry (ICP-MS). The flash of ions due to the ionisation of a thorium colloidal particle in the plasma torch can be detected and measured in a time scan for (232)Th (+ ) or (248)[ThO] (+ ) according to the sensitivity required by the mass spectrometer. The peaks of the recorded intensity of the MS signal can be analysed as a function of the particle size or fraction of the studied element in the colloid phase. The frequency of the flashes is directly proportional to the concentration of particles in the colloidal suspension. After discussing Th colloid detection, on the basis of the intensity of the ion flashes generated in the plasma torch, tests were performed on thorium dioxide colloidal particles. This feasibility study also describes the experimental conditions and the limitation of the plasma design to detect thorium colloids in a single particle analysis mode down to about 10fg.

  10. Reduction of plyatomic ion interferences in indictively coupled plasma mass spectrometry with cryogenic desolvation

    Energy Technology Data Exchange (ETDEWEB)

    Alves, L.C.

    1993-09-01

    A desolvation scheme for introducing aqueous and organic samples into an argon inductively coupled plasma is described; the aerosol generated by nebulizer is heated (+140 C) and cooled ({minus}80 C) repeatedly, and the dried aerosol is then injected into the mass spectrometer. Polyatomic ions are greatly suppressed. This scheme was validated with analysis of seawater and urine reference samples. Finally, the removal of organic solvents by cryogenic desolvation was studied.

  11. Determination of diclofenac concentrations in human plasma using a sensitive gas chromatography mass spectrometry method

    OpenAIRE

    2016-01-01

    Background A gas chromatography mass spectrometry (GCMS) method for the determination of diclofenac in human plasma has been developed and validated. Results This method utilizes hexane which is a relatively less toxic extraction solvent compared to heptane and benzene. In addition, phosphoric acid and acetone were added to the samples as deproteination agents, which increased the recovery of diclofenac. These revised processes allow clean extraction and near-quantitative recovery of analyte ...

  12. Determination of diclofenac concentrations in human plasma using a sensitive gas chromatography mass spectrometry method

    OpenAIRE

    Shah, Iltaf; Barker, James; Naughton, Declan P; Barton, Stephen J.; Ashraf, Syed Salman

    2016-01-01

    Background\\ud A gas chromatography mass spectrometry (GCMS) method for the determination of diclofenac in human plasma has been developed and validated.\\ud \\ud Results\\ud This method utilizes hexane which is a relatively less toxic extraction solvent compared to heptane and benzene. In addition, phosphoric acid and acetone were added to the samples as deproteination agents, which increased the recovery of diclofenac. These revised processes allow clean extraction and near-quantitative recover...

  13. Human Plasma N-Glycoproteome Analysis by Immunoaffinity Subtraction, Hydrazide Chemistry, and Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Tao; Qian, Weijun; Gritsenko, Marina A.; Camp, David G.; Monroe, Matthew E.; Moore, Ronald J.; Smith, Richard D.

    2005-12-01

    The enormous complexity, wide dynamic range of relative protein abundance of interest (over 10 orders of magnitude), and tremendous heterogeneity (due to post-translational modifications, such as glycosylation) of the human blood plasma proteome severely challenges the capabilities of existing analytical methodologies. We describe here the comprehensive analysis of human plasma N-glycoproteins using the combination of immunoaffinity subtraction and glycoprotein capture to reduce both the protein concentration range and the overall sample complexity. Six high-abundance plasma proteins were simultaneously removed using a pre-packed, immobilized antibody column. N-linked glycoproteins were then captured from the depleted plasma using hydrazide resin, enzymatically digested, and the bound, N-linked glycopeptides were released using peptide-N-glycosidase F. Following strong cation exchange (SCX) fractionation, the deglycosylated peptides were analyzed by reversed-phase capillary liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). A total of 2140 different N-glycopeptides were confidently identified using stringent criteria, covering 371 non-redundant N-glycoproteins with the majority of them being extracellular or membrane proteins. The strategy significantly improved the detection, enabling the identification of a number of low-abundance proteins, exemplified by interleukin-1 receptor antagonist protein ({approx}200 pg/mL), cathepsin L ({approx}1 ng/mL), and transforming growth factor beta 1 ({approx}2 ng/mL). A total of 712 N-glycosylation sites were identified and the confidence of these site identifications was further validated by accurate mass measurements using high resolution liquid chromatography coupled to Fourier transform ion cyclotron resonance mass spectrometry (LC-FTICR). This study provides the basis for future high-throughput measurements using the accurate mass and time tag approach.

  14. Imaging gold nanoparticles in mouse liver by laser ablation inductively coupled plasma mass spectrometry

    OpenAIRE

    Li, Qing; Wang, Zheng; Mo, Jiamei; Zhang, Guoxia; Chen, Yirui; Huang, Chuchu

    2017-01-01

    Imaging the size distribution of metal nanoparticles (NPs) in a tissue has important implications in terms of evaluating NP toxicity. Microscopy techniques used to image tissue NPs are limited by complicated sample preparation or poor resolution. In this study, we developed a laser ablation (LA) system coupled to single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) for quantitative imaging of gold (G)NPs in tissue samples. In this system, GNPs were ablated but did not disi...

  15. Plasma free and total carnitine measured in children by tandem mass spectrometry

    OpenAIRE

    J.H. Osorio; Pourfarzam, M.

    2002-01-01

    Free and total carnitine quantification is important as a complementary test for the diagnosis of unusual metabolic diseases, including fatty acid degradation disorders. The present study reports a new method for the quantification of free and total carnitine in dried plasma specimens by isotope dilution electrospray tandem mass spectrometry with sample derivatization. Carnitine is determined by looking for the precursor of ions of m/z = 103 of N-butylester derivative, and the method is valid...

  16. Analysis of estrogens and androgens in postmenopausal serum and plasma by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Wang, Qingqing; Bottalico, Lisa; Mesaros, Clementina; Blair, Ian A

    2015-07-01

    Liquid chromatography-selected reaction monitoring/mass spectrometry-based methodology has evolved to the point where accurate analyses of trace levels of estrogens and androgens in postmenopausal serum and plasma can be accomplished with high precision and accuracy. A suite of derivatization procedures has been developed, which together with modern mass spectrometry instrumentation provide investigators with robust and sensitive methodology. Pre-ionized derivatives are proving to be useful as they are not subject to suppression of the electrospray signal. Postmenopausal women with elevated plasma or serum estrogens are thought to be at increased risk for breast and endometrial cancer. Therefore, significant advances in risk assessment should be possible now that reliable methodology is available. It is also possible to conduct analyses of multiple estrogens in plasma or serum. Laboratories that are currently employing liquid chromatography/mass spectrometry methodology can now readily implement this strategy. This will help conserve important plasma and serum samples available in Biobanks, as it will be possible to conduct high sensitivity analyses using low initial sample volumes. Reported levels of both conjugated and non-conjugated estrogen metabolites are close to the limits of sensitivity of many assays to date, urging caution in the interpretation of these low values. The analysis of serum androgen precursors in postmenopausal women has not been conducted routinely in the past using liquid chromatography/mass spectrometry methodology. Integration of serum androgen levels into the panel of metabolites analyzed could provide additional information for assessing cancer risk and should be included in the future.

  17. Identification of novel circulating coffee metabolites in human plasma by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Redeuil, Karine; Smarrito-Menozzi, Candice; Guy, Philippe; Rezzi, Serge; Dionisi, Fabiola; Williamson, Gary; Nagy, Kornél; Renouf, Mathieu

    2011-07-22

    This study reports a liquid chromatography-mass spectrometry method for the detection of polyphenol-derived metabolites in human plasma without enzymatic treatment after coffee consumption. Separation of available standards was achieved by reversed-phase ultra performance liquid chromatography and detection was performed by high resolution mass spectrometry in negative electrospray ionization mode. This analytical method was then applied for the identification and relative quantification of circulating coffee metabolites. A total of 34 coffee metabolites (mainly reduced, sulfated and methylated forms of caffeic acid, coumaric acid, caffeoylquinic acid and caffeoylquinic acid lactone) were identified based on mass accuracy (<4 ppm for most metabolites), specific fragmentation pattern and co-chromatography (when standard available). Among them, 19 circulating coffee metabolites were identified for the first time in human plasma such as feruloylquinic acid lactone, sulfated and glucuronidated forms of feruloylquinic acid lactone and sulfated forms of coumaric acid. Phenolic acid derivatives such as dihydroferulic acid, dihydroferulic acid 4'-O-sulfate, caffeic acid 3'-O-sulfate, dimethoxycinnamic acid, dihydrocaffeic acid and coumaric acid O-sulfate appeared to be the main metabolites circulating in human plasma after coffee consumption. The described method is a sensitive and reliable approach for the identification of coffee metabolites in biological fluids. In future, this analytical method will give more confidence in compound identification to provide a more comprehensive assessment of coffee polyphenol bioavailability studies in humans.

  18. Ambient low temperature plasma etching of polymer films for secondary ion mass spectrometry molecular depth profiling.

    Science.gov (United States)

    Muramoto, Shin; Staymates, Matthew E; Brewer, Tim M; Gillen, Greg

    2012-12-18

    The feasibility of a low temperature plasma (LTP) probe as a way to prepare polymer bevel cross sections for secondary ion mass spectrometry (SIMS) applications was investigated. Poly(lactic acid) and poly(methyl methacrylate) films were etched using He LTP, and the resulting crater walls were depth profiled using time-of-flight secondary ion mass spectrometry (ToF-SIMS) to examine changes in chemistry over the depth of the film. ToF-SIMS results showed that while exposure to even 1 s of plasma resulted in integration of atmospheric nitrogen and contaminants to the newly exposed surface, the actual chemical modification to the polymer backbone was found to be chemistry-dependent. For PLA, sample modification was confined to the top 15 nm of the PLA surface regardless of plasma exposure dose, while measurable change was not seen for PMMA. The confinement of chemical modification to 15 nm or less of the top surface suggests that LTP can be used as a simple method to prepare cross sections or bevels of polymer thin films for subsequent analysis by surface-sensitive molecular depth profiling techniques such as SIMS, X-ray photoelectron spectroscopy (XPS), and other spatially resolved mass spectrometric techniques.

  19. Determination of Candesartan in Human Plasma with Liquid Chromatography - Tandem Mass Spectrometry.

    Science.gov (United States)

    Forjan, Vanja; Cvitkovič Maričič, Lea; Prosen, Helena; Brodnjak Vončina, Darinka

    2016-01-01

    A sensitive, specific and rapid liquid chromatography - tandem mass spectrometry method was developed and validated for the determination of candesartan in human plasma. Analyte was separated from endogenous components present in plasma by solid phase extraction. Chromatographic separation was performed on Gemini C18 analytical column using mobile phase acetonitrile - 5 mM ammonium formate pH 2 (90:10, v/v) at flow rate of 0.3 mL/min. For detection, tandem mass spectrometry in SRM mode with positive electrospray ionization was used. The mass transitions m/z 441.1 > 263.1 and 445.1 > 267.1 were used to determine candesartan by using candesartan-d4 as an internal standard. After development, the method was validated according to the requirements of EMA regulatory guidelines in the concentration range 1 - 400 ng/ml in human plasma. Limit of quantification (LLOQ) was 1 ng/ml. The developed and validated method proved to be very fast and reproducible and was therefore successfully implemented in pharmacokinetic and bioequivalence studies with large number of study samples.

  20. Myoglobin plasma level related to muscle mass and fiber composition: a clinical marker of muscle wasting?

    Science.gov (United States)

    Weber, Marc-André; Kinscherf, Ralf; Krakowski-Roosen, Holger; Aulmann, Michael; Renk, Hanna; Künkele, Annette; Edler, Lutz; Kauczor, Hans-Ulrich; Hildebrandt, Wulf

    2007-08-01

    Progressive muscle wasting is a central feature of cancer-related cachexia and has been recognized as a determinant of poor prognosis and quality of life. However, until now, no easily assessable clinical marker exists that allows to predict or to track muscle wasting. The present study evaluated the potential of myoglobin (MG) plasma levels to indicate wasting of large locomotor muscles and, moreover, to reflect the loss of MG-rich fiber types, which are most relevant for daily performance. In 17 cancer-cachectic patients (weight loss 22%) and 27 age- and gender-matched healthy controls, we determined plasma levels of MG and creatine kinase (CK), maximal quadriceps muscle cross-sectional area (CSA) by magnetic resonance imaging, muscle morphology and fiber composition in biopsies from the vastus lateralis muscle, body cell mass (BCM) by impedance technique as well as maximal oxygen uptake (VO(2)max). In cachectic patients, plasma MG, muscle CSA, BCM, and VO(2)max were 30-35% below control levels. MG showed a significant positive correlation to total muscle CSA (r = 0.65, p max as an important functional readout. CK plasma levels appear to be less reliable because prolonged increases are observed in even subclinical myopathies or after exercise. Notably, cancer-related muscle wasting was not associated with increases in plasma MG or CK in this study.

  1. Mass and energy analysis of the ions in a plasma flood system

    Energy Technology Data Exchange (ETDEWEB)

    Wooding, A.C. [Institute of Materials Research, University of Salford, Salford M54WT (United Kingdom); Armour, D.G. [Institute of Materials Research, University of Salford, Salford M54WT (United Kingdom); Berg, J.A. van den [Institute of Materials Research, University of Salford, Salford M54WT (United Kingdom)]. E-mail: j.a.vandenberg@salford.ac.uk; Holmes, A.J.T. [Marcham Scientific, Hungerford, Berks RG17 0LH (United Kingdom); Burgess, C. [Applied Materials UK Ltd., Foundry Lane, Horsham, West Sussex RH13 5PX (United Kingdom); Goldberg, R.D. [Applied Materials UK Ltd., Foundry Lane, Horsham, West Sussex RH13 5PX (United Kingdom)

    2005-08-01

    Plasma flood systems, capable of providing a copious supply of electrons are used in ion implanters to control wafer charging and provide effective space charge neutralisation of the ion beam in the post-analysis/post-deceleration section of the beamline. Under appropriate conditions the plasma from the flood system interacts with the ion beam and this bridging leads to an enhanced beam transport efficiency in the final critical stage of the beamline. The effectiveness of this process depends on the properties of the plasma emanating from the system. In this study, a plasma analyser comprising a double hemi-spherical electrostatic energy analyser and a quadrupole mass spectrometer, was used to measure the energy distributions of all the ion species leaving a magnetically confined argon plasma, generated in the discharge chamber of a conventional flood neutraliser. The energy distributions extended to surprisingly high energies and the peak structures depended strongly on discharge voltage, discharge current and gas pressure. The nature of these dependencies was complex with both the pressure and arc current affecting the way in which the ion energy distributions depended on arc voltage. In all cases, multiply charged ions played a significant role in determining the nature of the ion energy distributions.

  2. A method for studies on interactions between a gold-based drug and plasma proteins based on capillary electrophoresis with inductively coupled plasma mass spectrometry detection

    DEFF Research Database (Denmark)

    Nguyen, Tam T T N; Østergaard, Jesper; Gammelgaard, Bente

    2015-01-01

    An analytical method based on capillary electrophoresis (CE) and inductively coupled plasma mass spectrometry (ICP-MS) detection was developed for studies on the interaction of gold-containing drugs and plasma proteins using auranofin as example. A detection limit of 18 ng/mL of auranofin...... was the major auranofin-interacting protein in plasma. The CE-ICP-MS method is proposed as a novel approach for kinetic studies of the interactions between gold-based drugs and plasma proteins. Graphical Abstract Development of a CE-ICP-MS based method allows for studies on interaction of the gold containing...

  3. Characterization of Plasma Membrane Proteins from Ovarian Cancer Cells Using Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    David L. Springer

    2004-01-01

    Full Text Available To determine how the repertoire of plasma membrane proteins change with disease state, specifically related to cancer, several methods for preparation of plasma membrane proteins were evaluated. Cultured cells derived from stage IV ovarian tumors were grown to 90% confluence and harvested in buffer containing CHAPS detergent. This preparation was centrifuged at low speed to remove insoluble cellular debris resulting in a crude homogenate. Glycosylated proteins in the crude homogenate were selectively enriched using lectin affinity chromatography. The crude homogenate and the lectin purified sample were prepared for mass spectrometric evaluation. The general procedure for protein identification began with trypsin digestion of protein fractions followed by separation by reversed phase liquid chromatography that was coupled directly to a conventional tandem mass spectrometer (i.e. LCQ ion trap. Mass and fragmentation data for the peptides were searched against a human proteome data base using the informatics program SEQUEST. Using this procedure 398 proteins were identified with high confidence, including receptors, membrane-associated ligands, proteases, phosphatases, as well as structural and adhesion proteins. Results indicate that lectin chromatography provides a select subset of proteins and that the number and quality of the identifications improve as does the confidence of the protein identifications for this subset. These results represent the first step in development of methods to separate and successfully identify plasma membrane proteins from advanced ovarian cancer cells. Further characterization of plasma membrane proteins will contribute to our understanding of the mechanisms underlying progression of this deadly disease and may lead to new targeted interventions as well as new biomarkers for diagnosis.

  4. Switched ferroelectric plasma ionizer (SwiFerr) for ambient mass spectrometry.

    Science.gov (United States)

    Neidholdt, Evan L; Beauchamp, J L

    2011-01-01

    We present the implementation of a switched ferroelectric plasma ionizer (SwiFerr) for ambient analysis of trace substances by mass spectrometry. The device utilizes the ferroelectric properties of barium titanate (BaTiO(3)) to take advantage of the high electric field resulting from polarization switching in the material. The source comprises a [001]-oriented barium titanate crystal (5 × 5 × 1 mm) with a metallic rear electrode and a metallic grid front electrode. When a high voltage AC waveform is applied to the rear electrode to switch polarization, the resulting electric field on the face of the crystal promotes electron emission and results in plasma formation between the crystal face and the grounded grid at ambient pressure. Interaction with this plasma and the resulting reagent ions effects ionization of trace neutrals. The source requires less than 1 W of power to operate under most circumstances, ionizes molecules with acidic and basic functional groups easily, and has proven quite versatile for ambient analysis of both vapor phase and aspirated powdered solid samples. Ionization of vapor phase samples of the organics triethylamine, tripropylamine, tributylamine, and pyridine results in observation of the singly protonated species in the positive ion mass spectrum with sensitivity extending into the high ppb range. With acetic acid, deprotonated clusters dominate the negative ion mass spectrum. Aerodynamic sampling of powdered samples is used to record mass spectra of the pharmaceuticals loperamide and ibuprofen. Chemical signatures, including protonated loperamide and deprotonated ibuprofen, are observed for each drug. The robust, low power source lends itself easily to miniaturization and incorporation in field-portable devices used for the rapid detection and characterization of trace substances and hazardous materials in a range of different environments.

  5. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    Science.gov (United States)

    Montaser, A.

    This research follows a multifaceted approach, from theory to practice, to the investigation and development of novel helium plasmas, sample introduction systems, and diagnostic techniques for atomic and mass spectrometries. During the period January 1994 - December 1994, four major sets of challenging research programs were addressed that each included a number of discrete but complementary projects: (1) The first program is concerned with fundamental and analytical investigations of novel atmospheric-pressure helium inductively coupled plasmas (He ICPS) that are suitable for the atomization-excitation-ionization of elements, especially those possessing high excitation and ionization energies, for the purpose of enhancing sensitivity and selectivity of analytical measurements. (2) The second program includes simulation and computer modeling of He ICPS. The aim is to ease the hunt for new helium plasmas by predicting their structure and fundamental and analytical properties, without incurring the enormous cost for extensive experimental studies. (3) The third program involves spectroscopic imaging and diagnostic studies of plasma discharges to instantly visualize their prevailing structures, to quantify key fundamental properties, and to verify predictions by mathematical models. (4) The fourth program entails investigation of new, low-cost sample introduction systems that consume micro- to nanoliter quantity of sample solution in plasma spectrometries. A portion of this research involves development and applications of novel diagnostic techniques suitable for probing key fundamental properties of aerosol prior to and after injection into high-temperature plasmas. These efforts, still in progress, collectively offer promise of solving singularly difficult analytical problems that either exist now or are likely to arise in the future in the various fields of energy generation, environmental pollution, material science, biomedicine and nutrition.

  6. Nitrogen mass transfer models for plasma-based low-energy ion implantation

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Bocong; Wang, Kesheng; Zhang, Zhipeng; Che, Honglong; Lei, Mingkai, E-mail: mklei@dlut.edu.cn [Surface Engineering Laboratory, School of Materials Science and Engineering, Dalian University of Technology, Dalian 116024 (China)

    2015-03-15

    The nitrogen mass transfer process in plasma-based low-energy ion implantation (PBLEII) is theoretically and experimentally studied in order to explore the process mechanism of PBLEII and therefore to optimize the apparatus design and the process conditions. An electron cyclotron resonance (ECR) microwave discharge generates the nitrogen plasma with a high density of 10{sup 11}–10{sup 12} ions/cm{sup 3}, which diffuses downstream to the process chamber along the divergent magnetic field. The nitrogen ions in the plasma implant into the surface and transport to the matrix of an austenitic stainless steel under the low negative pulsed bias of −2 kV at a process temperature of 400 °C. A global plasma model is used to simulate the ECR microwave plasma discharge for a range of working pressures and microwave powers. The fluid models are adopted to calculate the plasma downstream diffusion, the sheath expansion and the low-energy ion implantation on the surface. A nonlinear kinetic discrete model is established to describe the nitrogen transport in the austenitic stainless steel and the results are compared with the experimental measurements. Under an average implantation current density of 0.3–0.6 mA/cm{sup 2}, the surface nitrogen concentration in the range from 18.5 to 29 at. % is a critical factor for the nitrogen transport in the AISI 304 austenitic stainless steel by PBLEII, which accelerates the implanted nitrogen diffusion inward up to 6–12 μm during a nitriding time of 4 h.

  7. Determination of moxonidine in human plasma by liquid chromatography-electrospray ionisation-mass spectrometry.

    Science.gov (United States)

    Zhao, Luhua; Ding, Li; Wei, Xin

    2006-01-23

    A sensitive and specific liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method has been developed and validated for the identification and quantification of moxonidine in human plasma. After the addition of clonidine-HCl, the internal standard (IS) and sodium hydrogen carbonate, plasma samples were extracted using 5 mL ethyl acetate. The compounds were separated on a Lichrospher ODS (5 microm, 250 mm x 4.6 mm) column using an elution system of 10 mmol/L ammonium acetate buffer-methanol (20:80 v/v) as the mobile phase. Analytes were determined using electrospary ionization in a single quadrupole mass spectrometer. LC-ESI-MS was performed in the selected-ion monitoring (SIM) mode using target ions at m/z: 242.2 for moxonidine and m/z: 230.1 for the IS. The method has shown to be sensitive and specific by testing six different blank plasma batches. Linearity was established for the range of concentrations 0.01976-9.88 ng/mL with a coefficient of correlation (r) of 0.9999. The lower limit of quantification (LOQ) was identifiable and reproducible at 0.01976 ng/mL. The method has been successfully applied to study the pharmacokinetics of moxonidine in healthy male Chinese volunteers.

  8. Determination of doxepin and desmethyldoxepin in human plasma using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Badenhorst, D; Sutherland, F C; de Jager, A D; Scanes, T; Hundt, H K; Swart, K J; Hundt, A F

    2000-05-26

    A sensitive method for the simultaneous determination of doxepin and its active metabolite desmethyldoxepin in plasma was established, using high-performance liquid chromatographic separation with tandem mass spectrometric detection. The samples were extracted with hexane-isoamyl alcohol, separated on a Phenomenex Luna C18 5 microm, 150x2.1 mm column with a mobile phase consisting of methanol-water-formic acid (600:400:0.5, v/v) at a flow-rate of 0.25 ml/min. Detection was achieved by a Perkin-Elmer API 2000 mass spectrometer at unit resolution in multiple reaction monitoring mode monitoring the transition of the protonated molecular ions m/z 280.2, 266.2 and 250.1 to the product ions m/z 107.1, 107.1 and 191.0 for analyte, metabolite and internal standard (benzoctamine-HCl), respectively. TurbolonSpray ionisation was used for ion production. The mean recovery for doxepin and desmethyldoxepin was 90% and 75%, respectively, with a lower limit of quantification at 0.320 ng/ml and 0.178 ng/ml for the analyte and its metabolite, respectively, using 0.5 ml plasma for extraction. This is the first assay method described for the simultaneous determination of doxepin and desmethyldoxepin in plasma using LC-MS-MS. The method is sensitive enough to be used in drug bioavailability studies with doxepin.

  9. Determination of tolperisone in human plasma by liquid chromatography/tandem mass spectrometry for clinical application.

    Science.gov (United States)

    Choi, Chang-Ik; Park, Jung-In; Lee, Hye-In; Lee, Yun-Jeong; Jang, Choon-Gon; Bae, Jung-Woo; Lee, Seok-Yong

    2012-12-12

    We have developed and validated a simple, rapid, and sensitive liquid chromatography analytical method employing tandem mass spectrometry (LC-MS/MS) for the determination of tolperisone, a centrally acting muscle relaxant, in human plasma. After liquid-liquid extraction with methyl t-butyl ether, chromatographic separation of tolperisone was performed using a reversed-phase Luna C(18) column (2.0mm×50mm, 5μm particles) with a mobile phase of 10mM ammonium formate buffer (pH 3.5) - methanol (12:88, v/v) and quantified by tandem mass detection in ESI positive ion mode. The flow rate of the mobile phase was 250μL/min and the retention times of tolperisone and the internal standard (IS, dibucaine) were both 0.6min. The calibration curves were linear over a range of 0.5-300ng/mL (r>0.999). The lower limit of quantification, using 200μL human plasma, was 0.5ng/mL. The mean accuracy and precision for intra- and inter-day validation of tolperisone were within acceptable limits. The LC-MS/MS method reported here showed improved sensitivity for quantification of tolperisone in human plasma compared with previously described analytical methods. Lastly, the validated method was successfully applied to a pharmacokinetic study in humans.

  10. High Resolution Studies of the Origins of Polyatomic Ions in Inductively Coupled Plasma-Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ferguson, Jill Wisnewski [Iowa State Univ., Ames, IA (United States)

    2006-01-01

    The inductively coupled plasma (ICP) is an atmospheric pressure ionization source. Traditionally, the plasma is sampled via a sampler cone. A supersonic jet develops behind the sampler, and this region is pumped down to a pressure of approximately one Torr. A skimmer cone is located inside this zone of silence to transmit ions into the mass spectrometer. The position of the sampler and skimmer cones relative to the initial radiation and normal analytical zones of the plasma is key to optimizing the useful analytical signal [1]. The ICP both atomizes and ionizes the sample. Polyatomic ions form through ion-molecule interactions either in the ICP or during ion extraction [l]. Common polyatomic ions that inhibit analysis include metal oxides (MO+), adducts with argon, the gas most commonly used to make up the plasma, and hydride species. While high resolution devices can separate many analytes from common interferences, this is done at great cost in ion transmission efficiency--a loss of 99% when using high versus low resolution on the same instrument [2]. Simple quadrupole devices, which make up the bulk of ICP-MS instruments in existence, do not present this option. Therefore, if the source of polyatomic interferences can be determined and then manipulated, this could potentially improve the figures of merit on all ICP-MS devices, not just the high resolution devices often utilized to study polyatomic interferences.

  11. Comprehensive Analysis of Low-Molecular-Weight Human Plasma Proteome Using Top-Down Mass Spectrometry.

    Science.gov (United States)

    Cheon, Dong Huey; Nam, Eun Ji; Park, Kyu Hyung; Woo, Se Joon; Lee, Hye Jin; Kim, Hee Cheol; Yang, Eun Gyeong; Lee, Cheolju; Lee, Ji Eun

    2016-01-01

    While human plasma serves as a great source for disease diagnosis, low-molecular-weight (LMW) proteome (mass spectrometry to analyze the LMW proteoforms present in four types of human plasma samples pooled from three healthy controls (HCs) without immunoaffinity depletion and with depletion of the top two, six, and seven high-abundance proteins. The LMW proteoforms were first fractionated based on molecular weight using gel-eluted liquid fraction entrapment electrophoresis (GELFrEE). Then, the GELFrEE fractions containing up to 30 kDa were subjected to nanocapillary-LC-MS/MS, and the high-resolution MS and MS/MS data were processed using ProSightPC 3.0. As a result, a total of 442 LMW proteins and cleaved products, including those with post-translational modifications and single amino acid variations, were identified. From additional comparative analysis of plasma samples without immunoaffinity depletion between HCs and colorectal cancer (CRC) patients via top-down approach, tens of LMW proteoforms, including platelet factor 4, were found to show >1.5-fold changes between the plasma samples of HCs and CRC patients, and six of the LMW proteins were verified by Western blot analysis.

  12. Detection of metals and metalloproteins in the plasma of stroke patients by mass spectrometry methods.

    Science.gov (United States)

    Kodali, Phanichand; Chitta, Karnakar R; Landero Figueroa, Julio A; Caruso, Joseph A; Adeoye, Opeolu

    2012-10-01

    Stroke is the leading cause of adult disability, worldwide. Metalloproteins and metals play key roles in epigenetic events in living organisms, including hypertension, the most important modifiable risk factor for stroke. Thus, metalloproteins may be important target biomarkers for disease diagnosis. The primary goal of this study was to assess metal containing proteins in blood plasma, detected by ICP-MS, followed by ESIMS for peptide/protein identification. We then compared the relative concentration differences between samples from patients with ischemic stroke, hemorrhagic stroke and stroke mimics. In 29 plasma samples (10 stroke mimics, 10 ischemic stroke and 9 hemorrhagic stroke patients) previously collected from patients who presented to the University of Cincinnati Emergency Department within 12 hours of symptom onset for a plasma banking project. For the metal associated protein study, Mg, Mn, Cu, Se concentrations were statistically different when compared between stroke mimics vs. ischemic stroke patients and ischemic stroke patients vs. hemorrhagic stroke patients. Pb concentrations were statistically different when compared between stroke mimics vs. ischemic stroke patients and Mo levels were statistically the same among the three groups. In addition, we also report concentration levels and preliminary correlation studies for total elemental analysis among the three sets of patients. This pilot study demonstrates that mass spectrometry methods may be highly valuable in detecting novel stroke biomarkers in blood plasma. Expanded studies are warranted to confirm these findings.

  13. Radio frequency plasma polymer coatings for affinity capture MALDI mass spectrometry.

    Science.gov (United States)

    Li, Meiling; Timmons, Richard B; Kinsel, Gary R

    2005-01-01

    Surface modification of MALDI probes is an attractive approach for combining bioaffinity isolation of targeted biomolecules with mass spectrometric analysis of the captured species. In this work, we demonstrate that a polymer thin film, produced by pulsed rf plasma polymerization of allylamine and deposited directly on a MALDI probe, can be subsequently biotinylated to develop a bioaffinity capture MALDI probe. The synthesis and characterization of the probe by XPS, FT-IR, and AFM is described, and the selective isolation of avidin from a three-component mixture of avidin, lysozyme, and cytochrome c is presented. These initial results offer encouragement for the further exploration of rf plasma polymer deposition as a novel approach for the development of on-probe affinity capture MALDI probes.

  14. Inductively coupled plasma mass spectrometry (ICP-MS)and its application in life sciences

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Inductively-coupled plasma mass spectrometry (ICP-MS) has made much progress since its birth in the late 1990s. This paper will give a rather systematic overview on the use of this technique in new devices and technologies related to plasma source, sample-introducing device and detecting spectrometer etc. In this overview, an emphasis will be put on the evaluation of the ICPMS technique in combination with a series of physical, chemical and biological techniques, such as laser ablation (LA), capillary electrophoresis (CE) and high performance liquid chromatograph (HPLC), along with their representative high accuracy and high sensitivity. Finally, comprehensive and fruitful applications of the ICP-MS and its combinative techniques in the detection of trace metallic elements and isotopes in complex biological and environmental samples will be revealed.

  15. Plasma lipid analysis by hydrophilic interaction liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Sonomura, Kazuhiro; Kudoh, Shinobu; Sato, Taka-Aki; Matsuda, Fumihiko

    2015-06-01

    A novel method for the analysis of endogenous lipids and related compounds was developed employing hydrophilic interaction liquid chromatography with electrospray ionization tandem mass spectrometry. A hydrophilic interaction liquid chromatography with carbamoyl stationary phase achieved clear separation of phosphatidylcholine, lysophosphatidylcholine, sphingomyelin, ceramide, and mono-hexsosyl ceramide groups with good peak area repeatability (RSD% 0.99). The established method was applied to human plasma assays and a total of 117 endogenous lipids were successfully detected and reproducibly identified. In addition, we investigated the simultaneous detection of small polar metabolites such as amino and organic acids co-existing in the same biological samples processed in a single analytical run with lipids. Our results show that hydrophilic interaction liquid chromatography is a useful tool for human plasma lipidome analysis and offers more comprehensive metabolome coverage.

  16. [Analysis of Trace Inorganic Elements in Castor Oil by Inductively Coupled Plasma Mass Spectrometry].

    Science.gov (United States)

    Li, Tan-ping; Xie, Hua-lin; Nie, Xi-du

    2015-10-01

    A method for the determination of Na, Mg, Si, P, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Cd, Hg and Pb in castor oil after direct dilution with ethanol by inductively coupled plasma mass spectrometry (ICP-MS) was established. The sample was diluted by ethanol before ICP-MS determination. The condensation and deposition of high concentrations of carbon in mass cone interface and ion lens, which will decrease the sensitivity of element analysis, were avoided effectively by introducing O2 to plasma. The mass spectral interferences were eliminated by octopole reaction system (ORS). The matrix effects were calibrated to using Sc, Ge, Rh and Ir as internal standard elements. Au standard solution, which could form amalgam alloy with Hg, was dropped to eliminate the memory effect of Hg. The results show that the correlation coefficient for analyte is no less than 0.999 5, the detection limits is in the range of 0.06 - 20.1 ng x L(-1), the recovery is in the range of 990.4% - 110.2%, and the RSD is less than 4.8%. This method was very fast, simple and accurate to simultaneously analyze multi-elements in castor oil.

  17. Field-assisted paper spray mass spectrometry for the quantitative evaluation of imatinib levels in plasma.

    Science.gov (United States)

    D'Aronco, Sara; Calandra, Eleonora; Crotti, Sara; Toffoli, Giuseppe; Marangon, Elena; Posocco, Bianca; Traldi, Pietro; Agostini, Marco

    Drug levels in patients' bloodstreams vary among individuals and consequently therapeutic drug monitoring (TDM) is fundamental to controlling the effective therapeutic range. For TDM purposes, different analytical approaches have been used, mainly based on immunoassay, liquid chromatography- ultraviolet, liquid chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods. More recently a matrix-assisted laser desorption/ionisation method has been proposed for the determination of irinotecan levels in the plasma of subjects under therapy and this method has been cross- validated by comparison with data achieved by LC-MS/MS. However, to reach an effective point-of-care monitoring of plasma drug concentrations, a TDM platform technology for fast, accurate, low-cost assays is required. In this frame, recently the use of paper spray mass spectrometry, which is becoming a popular and widely employed MS method, has been proposed. In this paper we report the results obtained by the development of a paper spray-based method for quantitative analysis in plasma samples of imatinib, a new generation of anticancer drug. Preliminary experiments showed that poor sensitivity, reproducibility and linear response were obtained by the "classical" paper spray set-up. In order to achieve better results, it was thought of interest to operate in presence of a higher and more homogeneous electrical field. For this aim, a stainless steel needle connected with the high voltage power supply was mounted below the paper triangle. Furthermore, in order to obtain valid quantitative data, we analysed the role of the different equilibria participating to the phenomena occurring in paper spray experiments, depending either on instrumental parameters or on the chemical nature of analyte and solvents. A calibration curve was obtained by spiking plasma samples containing different amounts of imatinib (1) with known amounts of deuterated imatinib (1d3) as

  18. Investigation of a measure of robustness in inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Makonnen, Yoseif; Beauchemin, Diane

    2015-01-01

    In industrial/commercial settings where operators often have minimal expertise in inductively coupled plasma (ICP) mass spectrometry (MS), there is a prevalent need for a response factor indicating robust plasma conditions, which is analogous to the Mg II/Mg I ratio in ICP optical emission spectrometry (OES), whereby a Mg II/Mg I ratio of 10 constitutes robust conditions. While minimizing the oxide ratio usually corresponds to robust conditions, there is no specific target value that is widely accepted as indicating robust conditions. Furthermore, tuning for low oxide ratios does not necessarily guarantee minimal matrix effects, as they really address polyatomic interferences. From experiments, conducted in parallel for both MS and OES, there were some element pairs of similar mass and very different ionization potential that were exploited for such a purpose, the rationale being that, if these elements were ionized to the same extent, then that could be indicative of a robust plasma. The Be II/Li I intensity ratio was directly related to the Mg II/Mg I ratio in OES. Moreover, the 9Be+/7Li+ ratio was inversely related to the CeO+/Ce+ and LaO+/La+ oxide ratios in MS. The effects of different matrices (i.e. 0.01-0.1 M Na) were also investigated and compared to a conventional argon plasma optimized for maximum sensitivity. The suppression effect of these matrices was significantly reduced, if not eliminated in the case of 0.01 M Na, when the 9Be+/7Li+ ratio was around 0.30 on the Varian 820 MS instrument. Moreover, a very similar ratio (0.28) increased robustness to the same extent on a completely different ICP-MS instrument (PerkinElmer NEXION). Much greater robustness was achieved using a mixed-gas plasma with nitrogen in the outer gas and either nitrogen or hydrogen as a sheathing gas, as the 9Be+/7Li+ ratio was then around 1.70. To the best of our knowledge, this is the first report on using a simple analyte intensity ratio, 9Be+/7Li+, to gauge plasma robustness.

  19. High Performance Liquid Chromatography Tandem Mass Spectrometry Assay for the Determination of Cobinamide in Pig Plasma

    Science.gov (United States)

    McCracken, Brent A.; Brittain, Matthew K.

    2015-01-01

    Liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been widely utilized for the analysis of compounds in biological matrices due to its selectivity and sensitivity. This study describes the application of an LC-MS/MS-based approach toward the analysis of cobinamide in Yorkshire pig plasma. The selectivity, accuracy, precision, recovery, linearity, range, carryover, sensitivity, matrix effect, interference, stability, reproducibility, and ruggedness of the method were investigated in pig plasma. The accuracy and precision of the method was determined to be within 10% over three different days over a range of concentrations (25–10,000 ng/mL) that spanned more than two orders of magnitude. The lower limit of quantitation (LLOQ) for dicyanocobinamide was determined to be 25 ng/mL in pig plasma. Carryover was acceptable, as the area response of the carryover blanks were ≤15% of the area response of the nearest LLOQ standard for the analyte, while it was nonexistent for the internal standard. Specificity was ensured using six different lots of pig plasma. While the matrix effects of dicyanocobinamide in plasma were enhanced, ginsenoside Rb1 experienced signal suppression under the described conditions. The absolute recovery results for both compounds were consistent, precise, and reproducibly lower than expected at ~60% for dicyanocobinamide and ~22% for ginsenoside Rb1, confirming that a matrix standard curve was required for accurate quantitation. Cobinamide was shown to be very stable in matrix at various storage conditions including room temperature, refrigerated, and frozen at time intervals of 20 hours, 4 days, and 60 days respectively. This method was demonstrated to be sensitive, reproducible, stable, and rugged, and it should be applicable to the analysis of cobinamide in other biological matrices and species. PMID:26540437

  20. Probing silicon substitution in molecular sieves by plasma desorption mass spectrometry

    Science.gov (United States)

    Van Stipdonk, M. J.; von Heimburg, S. L.; Schweikert, E. A.

    1998-10-01

    Plasma desorption was used to produce secondary ion mass spectra from samples of unsubstituted and substituted aluminum phosphate materials. The yield of fingerprint ions representative of silicon oxide solids indicates that the incorporation of silicon into the material during synthesis and following calcination occurs via the formation of silicon-rich islands. Complementary X-ray photoelectron data provide supporting evidence that the surface of the substituted aluminum phosphate material becomes silicon rich and phosphorus depleted. No changes in the unsubstituted and substituted material with respect to composition and phase were detected using powder X-ray diffraction.

  1. The effect of boron supplementation on lean body mass, plasma testosterone levels, and strength in male bodybuilders

    Science.gov (United States)

    Ferrando, A. A.; Green, N. R.

    1993-01-01

    The effect of boron supplementation was investigated in 19 male bodybuilders ages 20-27 years. Ten were given a 2.5-mg boron supplement while 9 were given a placebo every day for 7 weeks. Plasma total and free testosterone, plasma boron, lean body mass, and strength measurements were determined on Days 1 and 49 of the study. Plasma boron values were significantly (p bodybuilding can increase total testosterone, lean body mass, and strength in lesser trained bodybuilders, and that boron supplementation had no effect on these measures.

  2. Development and evaluation of magnesium oxide-based ceramics for chamber parts in mass-production plasma etching equipment

    Science.gov (United States)

    Kasashima, Yuji; Tsutsumi, Kota; Mitomi, Shinzo; Uesugi, Fumihiko

    2017-06-01

    In mass-production plasma etching equipment, the corrosion of ceramic chamber parts reduces the production yield of LSI and overall equipment effectiveness (OEE) owing to contamination, short useful life, and particle generation. Novel ceramics that can improve the production yield and OEE are highly required. We develop magnesium oxide (MgO)-based ceramics and evaluate them under mass-production plasma etching conditions. The results of this study indicate that the developed MgO-based ceramics with high mechanical properties and low electric resistivity have a higher resistance to corrosion in plasma etching using CF4 gas than Si and conventional ceramic materials such as aluminum oxide and yttrium oxide.

  3. Improvement in Thermal-Ionization Mass Spectrometry (TIMS) using Total Flash Evaporation (TFE) method for lanthanides isotope ratio measurements in transmutation targets

    Energy Technology Data Exchange (ETDEWEB)

    Mialle, S.; Gourgiotis, A.; Aubert, M.; Stadelmann, G.; Gautier, C.; Isnard, H. [Commissariat a l' Energie Atomique, CEA Saclay, DEN/DPC/SECR/LANIE, 91191 Gif sur Yvette (France); Chartier, F. [Commissariat a l' Energie Atomique, CEA Saclay, DEN/DPC, 91191 Gif sur Yvette (France)

    2011-07-01

    The experiments involved in the PHENIX french nuclear reactor to obtain precise and accurate data on the total capture cross sections of the heavy isotopes and fission products require isotopic ratios measurements with uncertainty of a few per mil. These accurate isotopic ratio measurements are performed with mass spectrometer equipped with multi-collector system. The major difficulty for the analyses of these actinides and fission products is the low quantity of the initial powder enclosed in steel container (3 to 5 mg) and the very low quantities of products formed (several {mu}g) after irradiation. Specific analytical developments are performed by Thermal Ionization Mass Spectrometry (TIMS) to be able to analyse several nanograms of elements with this technique. A specific method of acquisition named Total Flash Evaporation was adapted in this study in the case of lanthanide measurements for quantity deposited on the filament in the order of 2 ng and applied on irradiated fuel. To validate the analytical approach and discuss about the accuracy of the data, the isotopic ratios obtained by TIMS are compared with other mass spectrometric techniques such as Multiple-Collector Inductively Coupled Plasma Mass Spectrometer (MC-ICPMS). (authors)

  4. Liquid chromatography/electrospray ionization mass spectrometric characterization of Harpagophytum in equine urine and plasma.

    Science.gov (United States)

    Colas, Cyril; Garcia, Patrice; Popot, Marie-Agnès; Bonnaire, Yves; Bouchonnet, Stéphane

    2006-01-01

    A method has been developed for the analysis and characterization in equine urine and plasma of iridoid glycosides: harpagide, harpagoside and 8-para-coumaroyl harpagide, which are the main active principles of Harpagophytum, a plant with antiinflammatory properties. The method involves liquid chromatography coupled with positive electrospray ionization mass spectrometry. The addition of sodium or lithium chloride instead of formic acid in the eluting solvent has been studied in order to enhance the signal and to modify the ion's internal energy. Fragmentation pathways and associated patterns are proposed for each analyte. A comparison of three types of mass spectrometer: a 3D ion trap, a triple quadrupole and a linear ion trap, has been conducted. The 3D ion trap was selected for drug screening analysis whereas the linear ion trap was retained for identification and quantitation analysis.

  5. Role of the electron mass in damping chiral plasma instability in Supernovae and neutron stars

    Science.gov (United States)

    Grabowska, Dorota; Kaplan, David B.; Reddy, Sanjay

    2015-04-01

    We show that the nonzero electron mass plays a critical role in determining the magnetic properties of neutron stars by suppressing the generation of the chiral charge density needed to trigger a strong chiral plasma instability during the core collapse of supernovae. This instability has been proposed as a plausible mechanism for generating extremely large helical magnetic fields in neutron stars at their birth; the mechanism relies on the generation of a large nonequilibrium chiral charge density via electron capture reactions that selectively deplete left-handed electrons during core collapse and the early evolution of the protoneutron star. Our calculation shows that the electron chirality violation rate induced by Rutherford scattering, despite being suppressed by the smallness of the electron mass relative to the electron chemical potential, is still fast compared to the weak interaction electron capture rate. The resulting asymmetry between right- and left-handed electron densities is therefore unlikely to attain an astrophysically relevant magnitude.

  6. A Movable Mass Spectroscopy Sampling Apparatus for Measuring Spatial Distribution of Neutral Radicals in Silane Plasma

    Institute of Scientific and Technical Information of China (English)

    WANG Zhao-Kui; LIN Kui-Xun; LIN Xuan-Ying; QIU Gui-Ming; ZHU Zu-Song

    2005-01-01

    @@ A movable mass spectroscopy gas sampling apparatus has been established and a straight-line fit ofsilane depletion fraction f is proposed.The spatial density distributions of SiHn (n = 0-3) radicals in silane radio frequency glow discharge have been measured by a mass spectrometer.The experimental results demonstrate that the densities of the neutral radicals have the peak value near the middle position of electrodes, and the densities of SiH2 and SiHs are higher than those of Si and SiH in silane plasma.This reveals that SiH2 and SiH3 may be the primary precursors in forming the a-Si:H film.

  7. Determination of trace multi-elements in coal fly ash by inductively coupled plasma mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    XIE Hua-lin; TANG You-gen; LI Yu-jie; LI Li-bo

    2007-01-01

    The contents of Cr,Cu, Ni, As, Cd and Pb in coal fly ash were determined by a high resolution inductively coupled plasma mass spectrometry method.The sample digestions were performed in closed microwave vessels with HN03, HClO4 and HF.The optimum conditions for the determination were obtained.The applicability of the proposed method was validated by the analysis of coal fly ash reference material (NIST SRM 1633a). The results show that most of the spectral interferences can be avoided by measuring in the high resolution mode(maximum mass resolution R=9 000).The detection limit is from 0.05 to 0.21μg/g,and the precision is fine with relative standard deviation less than 4.3%.

  8. Liquid Chromatography-Electrospray Ionization Mass Spectrometry Method for Determination of Protopanaxadiol in Rat Plasma

    Institute of Scientific and Technical Information of China (English)

    WU Yi; TENG Guo-sheng; LIANG Yong-tao; ZHONG Da-fang; LIU Bing

    2009-01-01

    A simple, rapid and sensitive method for the determination of protopanaxadiol in rat plasma with ginse-noside Rh2 as internal standard was developed and validated. The analyte and internal standard were extracted from plasma with ether-dichloromethane(3:2, volume ratio) and then were analyzed by reversed-phase HPLC on a short Zorbax Extend C_(18) column(50 mm×2.1 mm, 3.5 μm i.d.) eluted with a mobile phase consisting of acetoni-trile/methanol 0.10 mmol/L ammonium acetate(45:45:10, volume ratio) at 0.4 mL/min. Detection was performed on an Applied Biosystems Sciex API 4000 mass spectrometer set at unit resolution in the multiple reaction monitoring mode. Electrospray ionization was used for ion production. The assay method shows linear over a range of 5-2000 ng/mL and intra- and inter-day precisions over this range were <10.0% with accuracy ranged from 86.3% to 114.1%. The limit of detection was 500 pg/mL in the plasma. The method was successfully applied to a preclinical pharmaco-kinetic study of protopanaxadiol(17.5 mg/kg) administered as a single oral dose.

  9. Simultaneous liquid chromatography-mass spectrometry quantification of cefixime and clavulanic acid in human plasma.

    Science.gov (United States)

    Dubala, Anil; Nagarajan, Janaki Sankarachari Krishnan; Vimal, Chandran Sathish; George, Renjith

    2015-01-01

    A simple and specific liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) assay method has been developed and fully validated for the simultaneous quantification of cefixime (CX) and clavulanic acid (CA) in human plasma. Analytes and internal standard were extracted from human plasma by a solid phase extraction technique using a Sam prep (3 mL, 100 mg) extraction cartridge. The extracted samples were chromatographed on a reverse phase C18 column using a mixture of methanol : acetonitrile : 2 mM ammonium acetate (pH 3.5) (25 : 25 : 50, v/v/v) as the mobile phase at a flow rate of 0.8 mL/min. Quantification of the analytes were carried out using single quadrupole LC-APCI-MS through selected ion monitoring at m/z 452 and 198, respectively, for CX and CA. The assay was linear over the concentration range of 0.05-10.0 and 0.1-10.0 μg/mL, respectively, for CX and CA. The mean plasma extraction recoveries of the CX and CA were found to be 95.20-96.27% and 94.67-95.58%, respectively. The method was successfully applied for the determination of pharmacokinetics of CX and CA after oral administration of single dosage CX/CA (200/125 mg) pill to the humans (n = 12).

  10. Bioimaging of metals by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS).

    Science.gov (United States)

    Becker, J Sabine; Zoriy, Miroslav; Matusch, Andreas; Wu, Bei; Salber, Dagmar; Palm, Christoph; Becker, J Susanne

    2010-01-01

    The distribution analysis of (essential, beneficial, or toxic) metals (e.g., Cu, Fe, Zn, Pb, and others), metalloids, and non-metals in biological tissues is of key interest in life science. Over the past few years, the development and application of several imaging mass spectrometric techniques has been rapidly growing in biology and medicine. Especially, in brain research metalloproteins are in the focus of targeted therapy approaches of neurodegenerative diseases such as Alzheimer's and Parkinson's disease, or stroke, or tumor growth. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) using double-focusing sector field (LA-ICP-SFMS) or quadrupole-based mass spectrometers (LA-ICP-QMS) has been successfully applied as a powerful imaging (mapping) technique to produce quantitative images of detailed regionally specific element distributions in thin tissue sections of human or rodent brain. Imaging LA-ICP-QMS was also applied to investigate metal distributions in plant and animal sections to study, for example, the uptake and transport of nutrient and toxic elements or environmental contamination. The combination of imaging LA-ICP-MS of metals with proteomic studies using biomolecular mass spectrometry identifies metal-containing proteins and also phosphoproteins. Metal-containing proteins were imaged in a two-dimensional gel after electrophoretic separation of proteins (SDS or Blue Native PAGE). Recent progress in LA-ICP-MS imaging as a stand-alone technique and in combination with MALDI/ESI-MS for selected life science applications is summarized.

  11. Afterglow of a microwave microstrip plasma as an ion source for mass spectrometry

    Science.gov (United States)

    Pfeuffer, Kevin P.; White, Allen; Broekaert, José A. C.; Hieftje, Gary M.

    2015-01-01

    A microwave-induced plasma that was previously used for optical emission spectrometry has been repurposed as an afterglow ion source for mass spectrometry. This compact microwave discharge, termed the microstrip plasma (MSP), is operated at 20-50 W and 2.45 GHz in helium at a flow of 300 mL/min. The primary background ions present in the afterglow are ionized and protonated water clusters. An exponential dilution chamber was used to introduce volatile organic compounds into the MSP afterglow and yielded limits of detection in the 40 ppb to 7 ppm range (v/v). A hydride-generation system was also utilized for detection of volatile hydride-forming elements (arsenic, antimony, tin) in the afterglow and produced limits of detection in the 10-100 ppb range in solution. The MSP afterglow was found capable of desorption and ionization of analyte species directly from a solid substrate, suggesting its use as an ion source for ambient desorption/ionization mass spectrometry.

  12. Sensitive quantification of omeprazole and its metabolites in human plasma by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Hofmann, Ute; Schwab, Matthias; Treiber, Gerd; Klotz, Ulrich

    2006-02-02

    A sensitive method was developed for the simultaneous determination of omeprazole and its major metabolites 5-hydroxyomeprazole and omeprazole sulfone in human plasma by HPLC-electrospray mass spectrometry. Following liquid-liquid extraction HPLC separation was achieved on a ProntoSil AQ, C18 column using a gradient with 10 mM ammonium acetate in water (pH 7.25) and acetonitrile. The mass spectrometer was operated in the selected ion monitoring mode using the respective MH(+) ions, m/z 346 for omeprazole, m/z 362 for 5-hydroxy-omeprazole and omeprazol-sulfone and m/z 300 for the internal standard (2-{[(3,5-dimethylpyridine-2-yl)methyl]thio}-1H-benzimidazole-5-yl)methanol. The limit of quantification (LOQ) achieved with this method was 5 ng/ml for 5-hydroxyomeprazole and 10 ng/ml for omeprazole and omeprazole-sulfone using 0.25 ml of plasma. Intra- and inter-assay variability was below 11% over the whole concentration range from 5 to 250 ng/ml for 5-hydroxyomeprazol and from 10 to 750 ng/ml for omeprazole and omeprazole-sulfone. The method was successfully applied to the determination of pharmacokinetic parameters of esomeprazole and the two major metabolites after a single dose and under steady state conditions.

  13. Minimally-invasive Laser Ablation Inductively Coupled Plasma Mass Spectrometry analysis of model ancient copper alloys

    Energy Technology Data Exchange (ETDEWEB)

    Walaszek, Damian [University of Warsaw, Faculty of Chemistry, Biological and Chemical Research Centre, Żwirki i Wigury 101, 02-089 Warszawa (Poland); Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Senn, Marianne; Wichser, Adrian [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Faller, Markus [Laboratory for Jointing Technology and Corrosion, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Wagner, Barbara; Bulska, Ewa [University of Warsaw, Faculty of Chemistry, Biological and Chemical Research Centre, Żwirki i Wigury 101, 02-089 Warszawa (Poland); Ulrich, Andrea [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland)

    2014-09-01

    This work describes an evaluation of a strategy for multi-elemental analysis of typical ancient bronzes (copper, lead bronze and tin bronze) by means of laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS).The samples originating from archeological experiments on ancient metal smelting processes using direct reduction in a ‘bloomery’ furnace as well as historical casting techniques were investigated with the use of the previously proposed analytical procedure, including metallurgical observation and preliminary visual estimation of the homogeneity of the samples. The results of LA-ICPMS analysis were compared to the results of bulk composition obtained by X-ray fluorescence spectrometry (XRF) and by inductively coupled plasma mass spectrometry (ICPMS) after acid digestion. These results were coherent for most of the elements confirming the usefulness of the proposed analytical procedure, however the reliability of the quantitative information about the content of the most heterogeneously distributed elements was also discussed in more detail. - Highlights: • The previously proposed procedure was evaluated by analysis of model copper alloys. • The LA-ICPMS results were comparable to the obtained by means of XRF and ICPMS. • LA-ICPMS results indicated the usefulness of the proposed analytical procedure.

  14. Determination of mycophenolic acid in human plasma by ultra performance liquid chromatography tandem mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Vivek Upadhyay; Vikas Trivedi; Gaurang Shah; Manish Yadav; Pranav S. Shrivastav

    2014-01-01

    A simple, sensitive and high throughput ultra performance liquid chromatography tandem mass spectrometry method has been developed for the determination of mycophenolic acid in human plasma. The method involved simple protein precipitation of MPA along with its deuterated analog as an internal standard (IS) from 50 mL of human plasma. The chromatographic analysis was done on Acquity UPLC C18 (100mm*2.1mm,1.7mm) column under isocratic conditions using acetonitrile and 10 mM ammonium formate, pH 3.00 (75:25, v/v) as the mobile phase. A triple quadrupole mass spectrometer operating in the positive ionization mode was used for quantitation. In-source conversion of mycophenolic glucuronide metabolite to the parent drug was selectively controlled by suitable optimization of cone voltage, cone gas flow and desolvation temperature. The method was validated over a wide concentration range of 15–15000 ng/mL. The mean extraction recovery for the analyte and IS was 495%. Matrix effect expressed as matrix factors ranged from 0.97 to 1.02. The method was successfully applied to support a bioequivalence study of 500 mg mycophenolate mofetil tablet in 72 healthy subjects.

  15. Unique applications of solvent removal in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Minnich, M.

    1997-01-10

    Inductively coupled plasma mass spectrometry (ICP-MS) is the technique of choice for rapid, high precision, semiquantitative elemental and isotopic analysis for over 70 elements. Less than 20 years after the first mass spectrum was obtained by ICP-MS, this technique has applications in clinical chemistry, geochemistry, the semiconductor industry, the nuclear industry, environmental chemistry, and forensic chemistry. The determination of many elements, though, by ICP-MS is complicated by spectral interferences from background species, interelement spectral overlaps, and polyatomic ions of matrix elements. The emphasis of this thesis is the unique applications of solvent removal using cryogenic and membrane desolvation. Chapter 1 is a general introduction providing background information concerning the need for these methods and some information about the methods themselves. Chapter 5 discusses general conclusions and general observations pertaining to this work. Chapters 2, 3, and 4 have been processed separately for inclusion on the database. Chapter 2 describes a method to screen urine samples for vanadium using cryogenic desolvation. Chapter 3 compares solvent removal by cryogenic and membrane desolvation. Chapter 4 describes the use of cool plasma conditions for the determination of potassium in the presence of excess sodium by ICP-MS.

  16. Determination and pharmacokinetic studies of arecoline in dog plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Li, Bing; Zhou, Xu-Zheng; Li, Jian-Yong; Yang, Ya-Jun; Niu, Jian-Rong; Wei, Xiao-Juan; Liu, Xi-Wang; Li, Jin-Shan; Zhang, Ji-Yu

    2014-10-15

    A rapid and sensitive high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of arecoline concentration in dog plasma. Plasma sample was prepared by protein precipitation using n-hexane (containing 1% isoamyl alcohol) with β-pinene as an internal standard. Chromatographic separation was achieved on an Agilent C18 column (4.6×75mm, 3.5μm) using methanol: 5mM ammonium acetate as the mobile phase with isocratic elution. Mass detection was carried out using positive electrospray ionization in multiple reaction monitoring mode. The calibration curve for arecoline was linear over a concentration range of 2-500ng/mL. The intra-day and inter-day accuracy and precision were within the acceptable limits of ±10% at all concentrations. In summary, the LC-MS/MS method described herein was fully validated and successfully applied to the pharmacokinetic study of arecoline hydrobromide tablets in dogs after oral administration. Copyright © 2014. Published by Elsevier B.V.

  17. Determination of mycophenolic acid in human plasma by ultra performance liquid chromatography tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Vivek Upadhyay

    2014-06-01

    Full Text Available A simple, sensitive and high throughput ultra performance liquid chromatography tandem mass spectrometry method has been developed for the determination of mycophenolic acid in human plasma. The method involved simple protein precipitation of MPA along with its deuterated analog as an internal standard (IS from 50 µL of human plasma. The chromatographic analysis was done on Acquity UPLC C18 (100 mm×2.1 mm, 1.7 µm column under isocratic conditions using acetonitrile and 10 mM ammonium formate, pH 3.00 (75:25, v/v as the mobile phase. A triple quadrupole mass spectrometer operating in the positive ionization mode was used for quantitation. In-source conversion of mycophenolic glucuronide metabolite to the parent drug was selectively controlled by suitable optimization of cone voltage, cone gas flow and desolvation temperature. The method was validated over a wide concentration range of 15–15000 ng/mL. The mean extraction recovery for the analyte and IS was >95%. Matrix effect expressed as matrix factors ranged from 0.97 to 1.02. The method was successfully applied to support a bioequivalence study of 500 mg mycophenolate mofetil tablet in 72 healthy subjects.

  18. Molecularly imprinted polymers as selective adsorbents for ambient plasma mass spectrometry.

    Science.gov (United States)

    Cegłowski, Michał; Smoluch, Marek; Reszke, Edward; Silberring, Jerzy; Schroeder, Grzegorz

    2017-05-01

    The application of molecularly imprinted polymers (MIPs) as molecular scavengers for ambient plasma ionization mass spectrometry has been reported for the first time. MIPs were synthesized using methacrylic acid as functional monomer; nicotine, propyphenazone, or methylparaben as templates; ethylene glycol dimethacrylate as a cross-linker; and 2,2'-azobisisobutyronitrile as polymerization initiator. To perform ambient plasma ionization experiments, a setup consisting of the heated crucible, a flowing atmospheric-pressure afterglow (FAPA) plasma ion source, and a quadrupole ion trap mass spectrometer has been used. The heated crucible with programmable temperature allows for desorption of the analytes from MIPs structure which results in their direct introduction into the ion stream. Limits of detection, linearity of the proposed analytical procedure, and selectivities have been determined for three analytes: nicotine, propyphenazone, and methylparaben. The analytes used were chosen from various classes of organic compounds to show the feasibility of the analytical procedure. The limits of detections (LODs) were 10 nM, 10, and 0.5 μM for nicotine, propyphenazone, and methylparaben, respectively. In comparison with the measurements performed for the non-imprinted polymers, the values of LODs were improved for at least one order of magnitude due to preconcentration of the sample and reduction of background noise, contributing to signal suppression. The described procedure has shown linearity in a broad range of concentrations. The overall time of single analysis is short and requires ca. 5 min. The developed technique was applied for the determination of nicotine, propyphenazone, and methylparaben in spiked real-life samples, with recovery of 94.6-98.4%. The proposed method is rapid, sensitive, and accurate which provides a new option for the detection of small organic compounds in various samples. Graphical abstract The experimental setup used for analysis.

  19. Resonant laser ablation of metals detected by atomic emission in a microwave plasma and by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Cleveland, Danielle; Stchur, Peter; Hou, Xiandeng; Yang, Karl X; Zhou, Jack; Michel, Robert G

    2005-12-01

    It has been shown that an increase in sensitivity and selectivity of detection of an analyte can be achieved by tuning the ablation laser wavelength to match that of a resonant gas-phase transition of that analyte. This has been termed resonant laser ablation (RLA). For a pulsed tunable nanosecond laser, the data presented here illustrate the resonant enhancement effect in pure copper and aluminum samples, chromium oxide thin films, and for trace molybdenum in stainless steel samples, and indicate two main characteristics of the RLA phenomenon. The first is that there is an increase in the number of atoms ablated from the surface. The second is that the bandwidth of the wavelength dependence of the ablation is on the order of 1 nm. The effect was found to be virtually identical whether the atoms were detected by use of a microwave-induced plasma with atomic emission detection, by an inductively coupled plasma with mass spectrometric detection, or by observation of the number of laser pulses required to penetrate through thin films. The data indicate that a distinct ablation laser wavelength dependence exists, probably initiated via resonant radiation trapping, and accompanied by collisional broadening. Desorption contributions through radiation trapping are substantiated by changes in crater morphology as a function of wavelength and by the relatively broad linewidth of the ablation laser wavelength scans, compared to gas-phase excitation spectra. Also, other experiments with thin films demonstrate the existence of a distinct laser-material interaction and suggest that a combination of desorption induced by electronic transition (DIET) with resonant radiation trapping could assist in the enhancement of desorption yields. These results were obtained by a detailed inspection of the effect of the wavelength of the ablation laser over a narrow range of energy densities that lie between the threshold of laser-induced desorption of species and the usual analytical

  20. Large molecular mass materials in coal derived liquids by {sup 252}Cf-plasma and matrix assisted laser desorption mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Domin, M. [School of Pharmacy, London (United Kingdom). Dept. of Pharmaceutical and Biological Chemistry; Li, S.; Herod, A.A.; Larsen, J.W. [Lehigh Univ., Bethlehem, PA (United States). Dept. of Chemistry; Lazaro, M.J.; Kandiyoti, R. [Imperial College, London (United Kingdom). Dept. of Chemical Engineering and Chemical Technology

    1997-12-31

    A Point of Ayr coal extract, its hydrocracked product and the pyridine solubles/insolubles of a coal tar pitch have been examined using {sup 252}Cf-plasma desorption-mass spectrometry (PDMS) and matrix assisted laser desorption-mass spectrometry (MALDI-MS). Comparison of molecular masses (MMs) between the coal extract and its hydrocracked product by PDMS indicated ranges of masses in the product to be considerably smaller, with number and weight average MMs reduced by approximately a factor of two. MALDI-mass spectra of the same samples indicated a greater reduction in mass. Similar comparison of the pyridine soluble/insoluble fractions of the coal tar pitch showed smaller differences by PD-MS than by MALDI-MS. (orig.)

  1. [Determination of Heavy Metal Elements in Diatomite Filter Aid by Inductively Coupled Plasma Mass Spectrometry].

    Science.gov (United States)

    Nie, Xi-du; Fu, Liang

    2015-11-01

    This study established a method for determining Be, Cr, Ni, As, Cd, Sb, Sn, Tl, Hg and Pb, total 10 heavy metals in diatomite filter aid. The diatomite filter aid was digested by using the mixture acid of HNO₃ + HF+ H₃PO₄ in microwave system, 10 heavy metals elements were determined by inductively coupled plasma mass spectrometry (ICP-MS). The interferences of mass spectrometry caused by the high silicon substrate were optimized, first the equipment parameters and isotopes of test metals were selected to eliminate these interferences, the methane was selected as reactant gas, and the mass spectral interferences were eliminated by dynamic reaction cell (DRC). Li, Sc, Y, In and Bi were selected as the internal standard elements to correct the interferences caused by matrix and the drift of sensitivity. The results show that the detection limits for analyte is in the range of 3.29-15.68 ng · L⁻¹, relative standard deviations (RSD) is less than 4.62%, and the recovery is in the range of 90.71%-107.22%. The current method has some advantages such as, high sensitivity, accurate, and precision, which can be used in diatomite filter aid quality control and safety estimations.

  2. Effects of Ions Charge-Mass Ratio on Energy and Energy Spread of Accelerated Ions in Laser Driven Plasma

    Institute of Scientific and Technical Information of China (English)

    SANG Hai-Bo; DENG Shi-Qiang; XIE Bai-Song

    2013-01-01

    Effects of ions charge-mass ratio on energy and energy spread of accelerated ions in laser driven plasma are investigated in detail by proposing a simple double-layer model for a foil target driven by an ultrastrong laser.The radiation pressure acceleration mechanism plays an important role on the studied problem.For the ions near the plasma mirror,i.e.electrons layer,the dependence of ions energy on their charge-mass ratio is derived theoretically.It is found that the larger the charge-mass ratio is,the higher the accelerated ions energy gets.For those ions far away from the layer,the dependence of energy and energy spread on ions charge-mass ratio are also obtained by numerical performance.It exhibits that,as ions charge-mass ratio increases,not only the accelerated ions energy but also the energy spread will become large.

  3. ISEE-3 observations of a viscously-driven plasma sheet: magnetosheath mass and/or momentum transfer?

    Directory of Open Access Journals (Sweden)

    R. T. Mist

    Full Text Available A statistical analysis of data from the ISEE-3 distant tail campaign is presented. We investigate the mechanism driving slow, tailward flows observed in the plasma sheet. The possibility that these slow flows are driven by mass and/or momentum transfer across the distant tail magnetopause is explored. We establish that 40% of these flows could be driven by the transfer of approximately 4% of the magnetosheath momentum flux into the magnetotail. Current understanding of the Kelvin-Helmholtz instability suggests that this figure is consistent with the amount of momentum flux transfer produced by this mechanism. We also consider the possibility that these flows are solely driven by transferring magnetosheath plasma across the magnetopause. We find that there is sufficient mass observed on these field lines for this to be the sole driving mechanism for only 27% of the observed slow flows.

    Key words. Magnetospheric physics (magnetotail boundary layers; plasma convection; plasma sheet

  4. Rapid and Sensitive Method for Quantitative Determination of Lopinavir and Ritonavir in Human Plasma by Liquid Chromatography- Tandem Mass Specrtometry

    Directory of Open Access Journals (Sweden)

    G. A. Temghare

    2009-01-01

    Full Text Available A rapid and sensitive liquid chromatography-mass spectrometric (LC-MS-MS method for the simultaneous determination of lopinavir and ritonavir in human plasma using abacavir as internal standard has been developed and validated. Sample preparation of plasma involved solid phase extraction. Detection was performed using an Applied Biosystems Sciex API 2000 Mass spectrometer. The assay of lopinavir and ritonavir was linear over the range of 50 ng mL-1 to 20000 ng mL -1 and 20 ng mL -1 to 3000 ng mL-1 respectively with a precision of <15% and accuracy in the range of 85-115%. The limit of quantification in plasma for lopinavir and ritonavir was 50 ng mL -1 and 20 ng mL -1 respectively. The described method has the advantage of being rapid and easy and it could be applied in therapeutic monitoring of these drugs in human plasma

  5. Improved Cd determination in glasses by laser ablation inductively coupled plasma mass spectrometry using nitrogen as a matrix modifier

    Institute of Scientific and Technical Information of China (English)

    Qian Ni; Zhao Chu Hu; Zheng Yu Bao; Ya Feng Zhang

    2009-01-01

    The addition of 5-10 mL min-1 nitrogen to the central channel of plasma in Laser ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) increases the sensitivities of Cd by a factor of 3 and decreases oxide interferences by one order of magnitude, which allows the direct analysis of trace levels of Cd in glass samples. This simple method shows a great potential for the direct determination of Cd in various kinds of samples.

  6. The effect of boron supplementation on lean body mass, plasma testosterone levels, and strength in male bodybuilders

    Science.gov (United States)

    Ferrando, A. A.; Green, N. R.

    1993-01-01

    The effect of boron supplementation was investigated in 19 male bodybuilders ages 20-27 years. Ten were given a 2.5-mg boron supplement while 9 were given a placebo every day for 7 weeks. Plasma total and free testosterone, plasma boron, lean body mass, and strength measurements were determined on Days 1 and 49 of the study. Plasma boron values were significantly (p supplementation on any of the dependent variables. Both groups demonstrated significant increases in total testosterone, lean body mass, 1-RM squat, and 1-RM bench press. The findings suggest that 7 weeks of bodybuilding can increase total testosterone, lean body mass, and strength in lesser trained bodybuilders, and that boron supplementation had no effect on these measures.

  7. Stable isotope dilution analysis of hydrologic samples by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Garbarino, J.R.; Taylor, H.E.

    1987-01-01

    Inductively coupled plasma mass spectrometry is employed in the determination of Ni, Cu, Sr, Cd, Ba, Ti, and Pb in nonsaline, natural water samples by stable isotope dilution analysis. Hydrologic samples were directly analyzed without any unusual pretreatment. Interference effects related to overlapping isobars, formation of metal oxide and multiply charged ions, and matrix composition were identified and suitable methods of correction evaluated. A comparability study snowed that single-element isotope dilution analysis was only marginally better than sequential multielement isotope dilution analysis. Accuracy and precision of the single-element method were determined on the basis of results obtained for standard reference materials. The instrumental technique was shown to be ideally suited for programs associated with certification of standard reference materials.

  8. Filterless preconcentration, flow injection analysis and detection by inductively-coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    The influence of interferences in the analysis of elements by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly diminished by utilising a protocol of flow-injection analysis (FIA). The method is based on filterless preconcentration of metallic elements at the walls...... of a knotted reactor that was made of nylon tubings. In the load mode, the preconcentration was accomplished by precipitation of metallic species in alkaline-buffered carriers onto the inner walls of the hydrofilic tube. After a preconcen-tration period of 40-120 seconds using sample volumes of 4-10 m......L, the analyte was transferred by a FIAS 400 system to the ICP-MS detector by dissolving the species in an acidic carrier. The magnitude of the enrichment factor largely depended on the time of preconcentration, on the pH-value of the preconcentration buffer and on the pH-value of the samples. Enrichment factors...

  9. Determination of Trace Elements in High Purity Gold by High Resolution Inductively Coupled Plasma Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    XIE Hualin; HUANG Kelong; NIE Xidu; FU Liang

    2009-01-01

    Trace elements were determined in high purity gold by high resolution inductively coupled plasma mass spectrometry(HR-ICP-MS).Sample were decomposed by aqua regia.To overcome some potentially problematic spectral interference,measurements were acquired in both medium and high resolution modes.The matrix effects due to the presence of excessive HCl and Au were evaluated.The optimum conditions for the determination was tested and discussed.The standard addition method was employed for quantitative analysis.The detection limits range from 0.01 μg/g to 0.28 μg/g depending on the elements.The method is accurate,quick and convenient.It has been applied to the determination of trace elements in high purity gold with satisfactory results.

  10. Inductively coupled plasma mass spectrometry with hexapole collision cell: figures of merit and applications

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, S.F. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen]|[Radiation Physics and Chemistry Problems Inst., Minsk (Belarus); Becker, J.S. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen

    2000-11-01

    The use of gas-filled multipole collision cells represents important progress in ICP-MS instrumentation. It enables an increase in element sensitivity based on the improvement of ion transmission efficiency from near thermalization and collisional focusing of ions. In addition, gas-phase ion-molecule chemistry can be applied in order to reduce mass spectral interferences via charge transfer reaction of interfering ions with reaction gas or via fragmentation of interfering molecular ions by collision-induced dissociation. The application of a hexapole collision cell in quadrupole based ICP-MS (HEX-ICP-QMS) was studied systematically in order to characterize the analytical figures of merit of this approach. Additionally, the performance of different solution introduction systems as well as an inductively coupled plasma shielded torch was studied for use with HEX-ICP-QMS. (orig.)

  11. Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Ornatsky, Olga I; Kinach, Robert; Bandura, Dmitry R; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I; Nitz, Mark; Winnik, Mitchell A

    2008-01-01

    Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for elemental tagging of antibodies, immunostaining of live and fixed human leukemia cells, and preparation of samples for ICP-MS analysis. Quantitative analysis of surface antigens on model cell lines using a cocktail of seven lanthanide labeled antibodies demonstrated high specificity and concordance with conventional immunophenotyping.

  12. Continuous ice-core chemical analyses using inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    McConnell, Joseph R; Lamorey, Gregg W; Lambert, Steven W; Taylor, Kendrick C

    2002-01-01

    Impurities trapped in ice sheets and glaciers have the potential to provide detailed, high temporal resolution proxy information on paleo-environments, atmospheric circulation, and environmental pollution through the use of chemical, isotopic, and elemental tracers. We present a novel approach to ice-core chemical analyses in which an ice-core melter is coupled directly with both an inductively coupled plasma mass spectrometer and a traditional continuous flow analysis system. We demonstrate this new approach using replicated measurements of ice-core samples from Summit, Greenland. With this method, it is possible to readily obtain continuous, exactly coregistered concentration records for a large number of elements and chemical species at ppb and ppt levels and at unprecedented depth resolution. Such very-high depth resolution, multiparameter measurements will significantly expand the use of ice-core records for environmental proxies.

  13. Sensitive and specific liquid chromatographic-tandem mass spectrometric assay for barnidipine in human plasma.

    Science.gov (United States)

    Pawula, M; Watson, D; Teramura, T; Watanabe, T; Higuchi, S; Cheng, K N

    1998-11-20

    A sensitive and specific LC-MS-MS assay has been developed and validated for barnidipine (1-benzyl-3-pyrrolidinyl)methyl-2,6-dimethyl-4(m-nitrophenyl)-1,4-dihydr opyridine-3,5-dicarboxylate). The assay involves a simple and rapid solid-phase extraction procedure. Sample analysis was on a Spherisorb S3ODS2 100 mmX2 mm I.D. column, with a Finnigan TSQ 7000 mass spectrometer, using an electrospray interface and selective reaction monitoring (SRM). The intra- and inter-day precision and accuracy, determined as the coefficient of variation and relative error, respectively, were 11.8% or less. The limit of quantitation was 0.03 ng/ml, and the calibration was linear between 0.03 and 3.0 ng/ml. The method has been used successfully for the measurement of over two thousand human plasma samples from pharmacokinetic clinical trials.

  14. Heavy metals in aromatic spices by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Bua, Daniel Giuseppe; Annuario, Giovanni; Albergamo, Ambrogina; Cicero, Nicola; Dugo, Giacomo

    2016-09-01

    Objective of this study was to determine the content of Cd, Hg, As and Pb in common spices traded in the Italian market, using inductively coupled plasma-mass spectrometry (ICP-MS). The results were compared with the maximum limits established by the national Legislative Decree (LD) no. 107 implementing the Council Directive 88/388/EEC and by international organisations, such as Food and Agriculture Organization (FAO) and World Health Organization (WHO). Food safety for spices was assessed considering the tolerable weekly intake (TWI) and the provisional tolerable weekly intake (PTWI), respectively, for Cd and Hg and the 95% lower confidence limit of the benchmark dose of 1% extra risk (BMDL01) for As and Pb. Investigated elements in all samples were within the maximum limits as set by the national and international normative institutions. Nevertheless, the heavy metal content of some spices exceeded the PTWI, TWI and BMDL01, which needs attention when considering consumer's health.

  15. Determination of metals in composite diet samples by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Melnyk, Lisa Jo; Morgan, Jeffrey N; Fernando, Reshan; Pellizzari, Edo D; Akinbo, Olujide

    2003-01-01

    A study was conducted to evaluate the applicability of inductively coupled plasma-mass spectrometry (ICP-MS) techniques for determination of metals in composite diets. Aluminum, cadmium, chromium, copper, lead, manganese, nickel, vanadium, and zinc were determined by this method. Atmospheric pressure microwave digestion was used to solubilize analytes in homogenized composite diet samples, and this procedure was followed by ICP-MS analysis. Recovery of certified elements from standard reference materials ranged from 92 to 119% with relative standard deviations (RSDs) of 0.4-1.9%. Recovery of elements from fortified composite diet samples ranged from 75 to 129% with RSDs of 0-11.3%. Limits of detection ranged from 1 to 1700 ng/g; high values were due to significant amounts of certain elements naturally present in composite diets. Results of this study demonstrate that low-resolution quadrupole-based ICP-MS provides precise and accurate measurements of the elements tested in composite diet samples.

  16. Multiplex DNA assay based on nanoparticle probes by single particle inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Zhang, Shixi; Han, Guojun; Xing, Zhi; Zhang, Sichun; Zhang, Xinrong

    2014-04-01

    A multiplex DNA assay based on nanoparticle (NP) tags detection utilizing single particle mode inductively coupled plasma mass spectrometry (SP-ICP-MS) as ultrasensitive readout has been demonstrated in the article. Three DNA targets associated with clinical diseases (HIV, HAV, and HBV) down to 1 pM were detected by DNA probes labeled with AuNPs, AgNPs, and PtNPs via DNA sandwich assay. Single nucleotide polymorphisms in genes can also be effectively discriminated. Since our method is unaffected by the sample matrix, it is well-suited for diagnostic applications. Moreover, with the high sensitivity of SP-ICP-MS and the variety of NPs detectable by SP-ICP-MS, high-throughput DNA assay could be achieved without signal amplification or chain reaction amplification.

  17. Multielement Analysis of Deep-Sea Sediments by Inductively Coupled Plasma Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    XIA Ning; WU Zhaohui; GUO Dongfa; YAO De

    2008-01-01

    Marine sediments were dissolved by HNO3-HF-HCIO4 in a sealed container at low pressure; I-IF was evaporated in an open container and salts were dissolved in HCl by heating, then transferred to 2% HNO3 solution. A total of 45 elements, including Li, Be, So, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Cd, In, Sb, Cs, Ba, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Hf, Ta, W, TI, Pb, Bi, Th and U, were measured by inductively coupled plasma mass spectrometry (ICP-MS). Condi-tions and sample experiments showed that this procedure defines a good experimental method which has the advantages of clear interference, easy operation and reliable results. The concentrations of the 45 elements could be used for resource exploration, envi-ronmental assessment and academic research.

  18. Analysis of iodine in food samples by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Todorov, Todor I; Gray, Patrick J

    2016-01-01

    This work shows a method for the determination of iodine in a variety of food samples and reference materials using inductively coupled plasma-mass spectrometry (ICP-MS) following alkaline extraction. Optimisation of the addition of organic carbon showed that a minimum of 3% 2-propanol was necessary for a constant ratio of iodine to internal standard. The limit of quantification (LOQ), calculated as 30σ for the method, was 36 ng g(-1) in solid food samples. For method validation, seven standard reference materials (SRM) and 21 fortified food samples were used. The precision (%RSD) of the measurements was in the 2-7% range. Accuracies for the SRMs were 85-105%, while the fortified food samples showed 81-119% recoveries, including a number of samples fortified at 50% of the LOQ.

  19. Inductively Coupled Plasma: Fundamental Particle Investigations with Laser Ablation and Applications in Magnetic Sector Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Saetveit, Nathan Joe [Iowa State Univ., Ames, IA (United States)

    2008-01-01

    Particle size effects and elemental fractionation in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are investigated with nanosecond and femtosecond laser ablation, differential mobility analysis, and magnetic sector ICP-MS. Laser pulse width was found to have a significant influence on the LA particle size distribution and the elemental composition of the aerosol and thus fractionation. Emission from individual particles from solution nebulization, glass, and a pressed powder pellet are observed with high speed digital photography. The presence of intact particles in an ICP is shown to be a likely source of fractionation. A technique for the online detection of stimulated elemental release from neural tissue using magnetic sector ICP-MS is described. Detection limits of 1 μg L-1 or better were found for P, Mn, Fe, Cu, and Zn in a 60 μL injection in a physiological saline matrix.

  20. Determination of sodium cromoglycate in human plasma by liquid chromatography with tandem mass.

    Science.gov (United States)

    Liu, Xiao-yan; Qu, Ting-ting; Wang, Ben-jie; Wei, Chun-min; Yuan, Gui-yan; Zhang, Rui; Guo, Rui-chen

    2008-09-01

    A sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for the determination of sodium cromoglycate (SCG) in human plasma after a nasal dose of 10.4 mg sodium cromoglycate nasal spray, using pravastatin sodium as the internal standard. The method was validated over a linear range of 0.300-20.0 ng/mL. SCG and I.S. were extracted from 1.0 mL of heparinized plasma by C(18) solid-phase extraction cartridges using methanol as eluting solvent. The dried residue was reconstituted with 100 microL of mobile phase, and 10 microL was injected onto the LC-MS/MS system. Chromatographic separation was achieved on a C(18) column (250 x 4.6 mm i.d., 5 microm particle size) with a mobile phase of methanol-acetonitrile-water (containing 2 mmol/L ammonium acetate; 42.5:42.5:15, v/v/v) at a flow rate of 0.4 mL/min. The analytes were detected with a triple quad LC-MS/MS using ESI with positive ionization. Ions monitored in the multiple reaction monitoring mode were m/z 469.0 (precursor ion) to m/z 245.0 (product ion) for SCG and m/z 447.2 (precursor ion) to m/z327.1 (product ion) for pravastatin sodium (internal standard) The average recovery of SCG from human plasma was 94.88% and the lower limit of quantitation was 0.3 ng/mL. Results from a 3-day validation study demonstrated excellent precision and accuracy across the calibration range of 0.3-20 ng/mL. The method was successfully applied to the pharmacokinetic study of SCG in healthy Chinese volunteers.

  1. Determination of triapine, a ribonucleotide reductase inhibitor, in human plasma by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Feng, Ye; Kunos, Charles A; Xu, Yan

    2015-09-01

    Triapine is an inhibitor of ribonucleotide reductase (RNR). Studies have shown that triapine significantly decreases the activity of RNR and enhanced the radiation-mediated cytotoxicity in cervical and colon cancer. In this work, we have developed and validated a selective and sensitive LC-MS/MS method for the determination of triapine in human plasma. In this method, 2-[(3-fluoro-2-pyridinyl)methylene] hydrazinecarbothioamide (NSC 266749) was used as the internal standard (IS); plasma samples were prepared by deproteinization with acetonitrile; tripaine and the IS were separated on a Waters Xbridge Shield RP18 column (3.5 µm; 2.1 × 50 mm) using a mobile phase containing 25.0% methanol and 75.0% ammonium bicarbonate buffer (10.0 mM, pH 8.50; v/v); column eluate was monitored by positive turbo-ionspray tandem mass spectrometry; and quantitation of triapine was carried out in multiple-reaction-monitoring mode. The method developed had a linear calibration range of 0.250-50.0 ng/mL with correlation coefficient of 0.999 for triapine in human plasma. The IS-normalized recovery and the IS-normalized matrix factor of triapine were 101-104% and 0.89-1.05, respectively. The accuracy expressed as percentage error and precision expressed as coefficient of variation were ≤±6 and ≤8%, respectively. The validated LC-MS/MS method was applied to the measurement of triapine in patient samples from a phase I clinical trial.

  2. Delta34S measurements of sulfur by multicollector inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Clough, Robert; Evans, Peter; Catterick, Tim; Evans, E Hywel

    2006-09-01

    An accurate and precise method for the determination of delta34S measurements by multicollector inductively coupled plasma mass spectrometry has been developed. Full uncertainty budgets, taking into consideration all the uncertainties of the measurement process, have been calculated. The technique was evaluated by comparing measured values with a range of isotopically enriched sulfur solutions prepared by gravimetric addition of a 34S spike. The gravimetric and measured results exhibited a correlation of R2 >0.999. Repeat measurements were also made after adding Na (up to 420 microg g(-1)) and Ca (up to 400 microg g(-1)) salts to the sulfur standard. No significant deviations in the delta34S values were observed. The Russell correction expression (Ingle, C.; Sharp, B.; Horstwood, M.; Parrish, R.; Lewis, D. J. J. Anal. At. Spectrom. 2003, 18, 219) was used to correct for mass bias on the 34S/32S isotope amount ratio from the mass bias observed for the 30Si/28Si isotope amount ratio. Consistent compensation for instrumental mass bias was achieved. Resolution of the measured delta34S values was better than 1 per thousand after consideration of all uncertainty components. The technique was evaluated for practical applications by measurement of delta34S for a range of mineral waters by pneumatic nebulization sample introduction and the analysis of genuine and counterfeit pharmaceuticals using both laser ablation sample introduction and liquid chromatography. For the former two cases polyatomic interferences were resolved by operating the MC-ICPMS in medium resolution, while for the chromatographic analyses polyatomic interferences were minimized by the use of a membrane desolvator, allowing the instrument to be operated at a resolution of 400.

  3. Determination of strychnine and brucine in rat plasma using liquid chromatography electrospray ionization mass spectrometry.

    Science.gov (United States)

    Xu, Yanyan; Si, Duanyun; Liu, Changxiao

    2009-02-20

    A simple, sensitive and selective liquid chromatography-electrospray mass spectrometric (LC-ESI-MS) method was developed and validated for simultaneous determination of strychnine and brucine in rat plasma, using tacrine as the internal standard (IS). Sample preparation involved a liquid-liquid extraction of the analytes with n-hexane, dichloromethane and isopropanol (65:30:5, v/v/v) from 0.1mL of plasma. Chromatographic separation was carried out on a Waters C(18) column using a mobile phase of methanol-20mM ammonium formate-formic acid (32:68:0.68, v/v/v). Positive selected ion monitoring mode was used for detection of strychnine, brucine and the IS at m/z 335.2, m/z 395.2 and m/z 199.2, respectively. Linearity was obtained over the concentration range of 0.5-500ng/mL for strychnine and 0.1-100ng/mL for brucine. The lower limit of quantification was 0.5ng/mL and 0.1ng/mL for strychnine and brucine, respectively. The intra- and inter-day precision for both strychnine and brucine was less than 7.74%, and accuracy ranged from -4.38% to 2.21% at all QC levels. The method has been successfully applied to a pharmacokinetic study of processed Semen Strychni after oral administration to rats.

  4. Non-equilibrium quantum plasmas in scalar QED photon production, magnetic and Debye masses and conductivity

    CERN Document Server

    Boyanovsky, D; Simionato, M

    2000-01-01

    We study the generation of a non-equilibrium plasma in scalar QED with N charged scalar fields through spinodal instabilities in the case of a super cooled second order phase transition and parametric amplification when the order parameter oscillates with large amplitude around the minimum of the potential.The focus is to study the non-equilibrium electromagnetic properties of the plasma, such as photon production, electric and magnetic screening and conductivity. A novel kinetic equation is introduced to compute photon production far away from equilibrium in the large N limit and lowest order in the electromagnetic coupling.During the early stages of the dynamics the photon density grows exponentially and asymptotically the amplitude and frequency distribution becomes \\sim alpha m^2/[lambda^2 ømega^3] with lambda the scalar self-coupling and m the scalar mass.In the case of a phase transition,electric and magnetic fields are correlated on distances xi(t) \\sim sqrt{t} during the early stages and the power sp...

  5. Thermodynamic Structure of Collision-Dominated Expanding Plasma: Heating of Interplanetary Coronal Mass Injections

    Science.gov (United States)

    Liu, Y.; Richardson, J. D.; Belcher, J. W.; Kasper, J. C.; Elliott, H. A.

    2006-01-01

    We investigate the thermodynamic structure of interplanetary coronal mass ejections (ICMEs) using combined surveys of the ejecta between 0.3 and 20 AU. ICMEs are shown to have a moderate expansion in the solar wind compared with theoretical predictions. The expansion seems to be governed by a polytrope with gamma approx. 1.3 in this distance range. We find that Coulomb collisions are important contributors to the ion-ion equilibration process in the ICME plasma. The alpha-proton differential speed quickly drops to below 10 km/s due to strong Coulomb collisions. However, the two species of particles are far from thermal equilibrium with a temperature ratio T(sub alpha/T(sub p) = 4-6, suggestive of a preferential heating of alpha particles. The plasma heating rate as a function of heliocentric &stance required for the temperature profile is deduced by taking into account the expansion and energy transfer between protons and alphas via Coulomb collisions. The turbulence dissipation rate is also inferred from the inertial range power spectrum of magnetic fluctuations within ICMEs. Comparison of the turbulence dissipation rate with the required heating rate shows that turbulence dissipation seems sufficient to explain the ICME heating. Sources powering the turbulence are also investigated by examining the instabilities induced by temperature anisotropies and energy deposition by pickup ions.

  6. Screening of agrochemicals in foodstuffs using low-temperature plasma (LTP) ambient ionization mass spectrometry.

    Science.gov (United States)

    Wiley, Joshua S; García-Reyes, Juan F; Harper, Jason D; Charipar, Nicholas A; Ouyang, Zheng; Cooks, R Graham

    2010-05-01

    Low-temperature plasma (LTP) permits direct ambient ionization and mass analysis of samples in their native environment with minimal or no prior preparation. LTP utilizes dielectric barrier discharges (DBDs) to create a low power plasma which is guided by gas flow onto the sample from which analytes are desorbed and ionized. In this study, the potential of LTP-MS for the detection of pesticide residues in food is demonstrated. Thirteen multi-class agricultural chemicals were studied (ametryn, amitraz, atrazine, buprofezin, DEET, diphenylamine, ethoxyquin, imazalil, isofenphos-methyl, isoproturon, malathion, parathion-ethyl and terbuthylazine). To evaluate the potential of the proposed approach, LTP-MS experiments were performed directly on fruit peels as well as on fruit/vegetable extracts. Most of the agrochemicals examined displayed remarkable sensitivity in the positive ion mode, giving limits of detection (LOD) for the direct measurement in the low picogram range. Tandem mass spectrometry (MS/MS) was used to confirm identification of selected pesticides by using for these experiments spiked fruit/vegetable extracts (QuEChERS, a standard sample treatment protocol) at levels as low as 1 pg, absolute, for some of the analytes. Comparisons of the data obtained by direct LTP-MS were made with the slower but more accurate conventional LC-MS/MS procedure. Herbicides spiked in aqueous solutions were detectable at LODs as low as 0.5 microg L(-1) without the need for any sample preparation. The results demonstrate that ambient LTP-MS can be applied for the detection and confirmation of traces of agrochemicals in actual market-purchased produce and in natural water samples. Quantitative analysis was also performed in a few selected cases and displayed a relatively high degree of linearity over four orders of magnitude.

  7. Plasma free and total carnitine measured in children by tandem mass spectrometry.

    Science.gov (United States)

    Osorio, J H; Pourfarzam, M

    2002-11-01

    Free and total carnitine quantification is important as a complementary test for the diagnosis of unusual metabolic diseases, including fatty acid degradation disorders. The present study reports a new method for the quantification of free and total carnitine in dried plasma specimens by isotope dilution electrospray tandem mass spectrometry with sample derivatization. Carnitine is determined by looking for the precursor of ions of m/z = 103 of N-butylester derivative, and the method is validated by comparison with radioenzymatic assay. We obtained an inter- and intra-day assay coefficient of variation of 4.3 and 2.3, respectively. Free and total carnitine was analyzed in 309 dried plasma spot samples from children ranging in age from newborn to 14 years using the new method, which was found to be suitable for calculating reference age-related values for free and total carnitine (less than one month: 19.3 +/- 2.4 and 23.5 +/- 2.9; one to twelve months: 28.8 +/- 10.2 and 35.9 +/- 11.4; one to seven years: 30.7 +/- 10.3 and 38.1 +/- 11.9; seven to 14 years: 33.7 +/- 11.6, and 43.1 +/- 13.8 micro M, respectively). No difference was found between males and females. A significant difference was observed between neonates and the other age groups. We compare our data with reference values in the literature, most of them obtained by radioenzymatic assay. However, this method is laborious and time consuming. The electrospray tandem mass spectrometry method presented here is a reliable, rapid and automated procedure for carnitine quantitation.

  8. Plasma free and total carnitine measured in children by tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    J.H. Osorio

    2002-11-01

    Full Text Available Free and total carnitine quantification is important as a complementary test for the diagnosis of unusual metabolic diseases, including fatty acid degradation disorders. The present study reports a new method for the quantification of free and total carnitine in dried plasma specimens by isotope dilution electrospray tandem mass spectrometry with sample derivatization. Carnitine is determined by looking for the precursor of ions of m/z = 103 of N-butylester derivative, and the method is validated by comparison with radioenzymatic assay. We obtained an inter- and intra-day assay coefficient of variation of 4.3 and 2.3, respectively. Free and total carnitine was analyzed in 309 dried plasma spot samples from children ranging in age from newborn to 14 years using the new method, which was found to be suitable for calculating reference age-related values for free and total carnitine (less than one month: 19.3 ± 2.4 and 23.5 ± 2.9; one to twelve months: 28.8 ± 10.2 and 35.9 ± 11.4; one to seven years: 30.7 ± 10.3 and 38.1 ± 11.9; seven to 14 years: 33.7 ± 11.6, and 43.1 ± 13.8 µM, respectively. No difference was found between males and females. A significant difference was observed between neonates and the other age groups. We compare our data with reference values in the literature, most of them obtained by radioenzymatic assay. However, this method is laborious and time consuming. The electrospray tandem mass spectrometry method presented here is a reliable, rapid and automated procedure for carnitine quantitation.

  9. [Mass spectrometry analysis of blood plasma lipidome as method of disease diagnostics, evuation of effectiveness and optimization of drug therapy].

    Science.gov (United States)

    Lokhov, P G; Maslov, D L; Balashova, E E; Trifonova, O P; Medvedeva, N V; Torkhovskaya, T I; Ipatova, O M; Archakov, A I; Malyshev, P P; Kukharchuk, V V; Shestakova, E A; Shestakova, M V; Dedov, I I

    2015-01-01

    A new method for the analysis of blood lipid based on direct mass spectrometry of lipophilic low molecular weight fraction of blood plasma has been considered. Such technique allows quantification of hundreds of various types of lipids and this changes existing concepts on diagnostics of lipid disorders and related diseases. The versatility and quickness of the method significantly simplify its wide use. This method is applicable for diagnostics of atherosclerosis, diabetes, cancer and other diseases. Detalization of plasma lipid composition at the molecular level by means of mass spectrometry allows to assess the effectiveness of therapy and to optimize the drug treatment of cardiovascular diseases by phospholipid preparations.

  10. Multiplex bio-assay with inductively coupled plasma mass spectrometry: Towards a massively multivariate single-cell technology

    Energy Technology Data Exchange (ETDEWEB)

    Tanner, Scott D. [Institute of Biomaterials and Biomedical Engineering, University of Toronto, Room 407, 164 College Street, Toronto, Ontario, M5S 3G9 (Canada)], E-mail: sd.tanner@utoronto.ca; Ornatsky, Olga; Bandura, Dmitry R.; Baranov, Vladimir I. [Institute of Biomaterials and Biomedical Engineering, University of Toronto, Room 407, 164 College Street, Toronto, Ontario, M5S 3G9 (Canada)

    2007-03-15

    Recent progress in the development of massively multiplexed bioanalytical assays using element tags with inductively coupled plasma mass spectrometry detection is reviewed. Feasibility results using commercially available secondary immunolabeling reagents for leukemic cell lines are presented. Multiplex analysis of higher order is shown with first generation tag reagents based on functionalized carriers that bind lanthanide ions. DNA quantification using metallointercalation allows for cell enumeration or mitotic state differentiation. In situ hybridization permits the determination of cellular RNA. The results provide a feasibility basis for the development of a multivariate assay tool for individual cell analysis based on inductively coupled plasma mass spectrometry in a cytometer configuration.

  11. Investigations into the origins of polyatomic ions in inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    McIntyre, Sally M. [Iowa State Univ., Ames, IA (United States)

    2010-01-01

    An inductively coupled plasma-mass spectrometer (ICP-MS) is an elemental analytical instrument capable of determining nearly all elements in the periodic table at limits of detection in the parts per quadrillion and with a linear analytical range over 8-10 orders of magnitude. Three concentric quartz tubes make up the plasma torch. Argon gas is spiraled through the outer tube and generates the plasma powered by a looped load coil operating at 27.1 or 40.6 MHz. The argon flow of the middle channel is used to keep the plasma above the innermost tube through which solid or aqueous sample is carried in a third argon stream. A sample is progressively desolvated, atomized and ionized. The torch is operated at atmospheric pressure. To reach the reduced pressures of mass spectrometers, ions are extracted through a series of two, approximately one millimeter wide, circular apertures set in water cooled metal cones. The space between the cones is evacuated to approximately one torr. The space behind the second cone is pumped down to, or near to, the pressure needed for the mass spectrometer (MS). The first cone, called the sampler, is placed directly in the plasma plume and its position is adjusted to the point where atomic ions are most abundant. The hot plasma gas expands through the sampler orifice and in this expansion is placed the second cone, called the skimmer. After the skimmer traditional MS designs are employed, i.e. quadrupoles, magnetic sectors, time-of-flight. ICP-MS is the leading trace element analysis technique. One of its weaknesses are polyatomic ions. This dissertation has added to the fundamental understanding of some of these polyatomic ions, their origins and behavior. Although mainly continuing the work of others, certain novel approaches have been introduced here. Chapter 2 includes the first reported efforts to include high temperature corrections to the partition functions of the polyatomic ions in ICP-MS. This and other objections to preceeding

  12. Investigations into the origins of polyatomic ions in inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    McIntyre, Sally M. [Iowa State Univ., Ames, IA (United States)

    2010-01-01

    An inductively coupled plasma-mass spectrometer (ICP-MS) is an elemental analytical instrument capable of determining nearly all elements in the periodic table at limits of detection in the parts per quadrillion and with a linear analytical range over 8-10 orders of magnitude. Three concentric quartz tubes make up the plasma torch. Argon gas is spiraled through the outer tube and generates the plasma powered by a looped load coil operating at 27.1 or 40.6 MHz. The argon flow of the middle channel is used to keep the plasma above the innermost tube through which solid or aqueous sample is carried in a third argon stream. A sample is progressively desolvated, atomized and ionized. The torch is operated at atmospheric pressure. To reach the reduced pressures of mass spectrometers, ions are extracted through a series of two, approximately one millimeter wide, circular apertures set in water cooled metal cones. The space between the cones is evacuated to approximately one torr. The space behind the second cone is pumped down to, or near to, the pressure needed for the mass spectrometer (MS). The first cone, called the sampler, is placed directly in the plasma plume and its position is adjusted to the point where atomic ions are most abundant. The hot plasma gas expands through the sampler orifice and in this expansion is placed the second cone, called the skimmer. After the skimmer traditional MS designs are employed, i.e. quadrupoles, magnetic sectors, time-of-flight. ICP-MS is the leading trace element analysis technique. One of its weaknesses are polyatomic ions. This dissertation has added to the fundamental understanding of some of these polyatomic ions, their origins and behavior. Although mainly continuing the work of others, certain novel approaches have been introduced here. Chapter 2 includes the first reported efforts to include high temperature corrections to the partition functions of the polyatomic ions in ICP-MS. This and other objections to preceeding

  13. Liquid chromatography/tandem mass spectrometry assay for the quantification of troxerutin in human plasma.

    Science.gov (United States)

    Liu, Fei; Xu, Yu; Rui, Lei; Gao, Shu; Dong, Haijun; Guo, Qingxiang

    2006-01-01

    A simple, rapid, sensitive and specific liquid chromatography/tandem mass spectrometry method was developed and validated to quantify troxerutin in human plasma. The analyte and rutin, used as the internal standard, were analyzed on a Phenomenex Synergi Fusion RP column interfaced with a triple-quadrupole tandem mass spectrometer using positive electrospray ionization. Acetonitrile/water (20:80 v/v) was used as the isocratic mobile phase, with 0.1% formic acid in water. A simple sample preparation method of protein precipitation with perchloric acid was employed. The assay was linear over the concentration range 31.25-4000 pg/mL. Correlation coefficients generated by linear regression with a 1/x(2) weighting factor ranged from 0.9991 to 0.9996. The intra- and inter-day precision over the entire concentration range were less than 12.28%. The method was successfully applied to a pharmacokinetic study after oral administration of a 300 mg troxerutin drop pill to 18 healthy volunteers.

  14. Titan's Topside Ionospheric Composition: Cassini Plasma Spectrometer Ion Mass Spectrometer Measurements

    Science.gov (United States)

    Sittler, Edward; Hartle, Richard; Ali, Ashraf; Cooper, John; Lipatov, Alexander; Simpson, David; Sarantos, Menelaos; Chornay, Dennis; Smith, Todd

    2017-01-01

    We present ion composition measurements of Titan's topside ionosphere using both T9 and T15 Cassini Plasma Spectrometer (CAPS) Ion Mass Spectrometer (IMS) measurements. The IMS is able to make measurements of Titan's ionosphere due to ionospheric outflows as originally reported for the T9 flyby. This allows one to take advantage of the unique capabilities of the CAPS IMS which measures both the mass-per-charge (M/Q) of the ions and the fragments of the ions produced inside the sensor such as carbon, nitrogen and oxygen fragments. Specific attention will be given to such ions as NH4 +, N +, O +, CH4 +, CxHy +, and HCNH + ions as examples. The CAPS IMS uses a time-of-flight (TOF) technique which accelerates ions up to 14.6 kV, so they can pass through ultra-thin carbon foils. Neutral fragments are used to measure the ion M/Q and positive fragments to measure the atomic components. We preliminarily find, by using IMS measurements of T9 and T15 ionospheric outflows, evidence for methane group ions, nitrogen ions, ammonium ions, water group ions and CnHm + ions with n = 2, 3, and 4 within Titan's topside ionosphere. E.C. Sittler acknowledges support at Goddard Space Flight Center by the CAPS Cassini Project from JPL funds under contract # NAS703001TONMO711123/1405851.

  15. Identification of organically associated trace elements in wood and coal by inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Richaud, R.; Lazaro, M.J.; Lachas, H.; Miller, B.B.; Herod, A.A.; Dugwell, D.R.; Kandiyoti, R. [Imperial College of Science, Technology and Medicine, London (United Kingdom). Dept. of Chemical Engineering and Chemical Technology

    2000-07-01

    1-Methyl-2-pyrrolidinone (NMP) was used to extract samples of wood (forest residue) and coal; the extracts were analysed by inductively coupled plasma mass spectrometry (ICP-MS) using two different sample preparation methods, in order to identify trace elements associated with the organic part of the samples. A sample of fly ash was similarly extracted and analysed. Size exclusion chromatograms of the extracts indicated the presence of significant amounts of large molecular mass materials ({gt} 1000 {mu}) in the biomass and coal extracts but not in the ash extract. Trace element analyses were carried out using ICP-MS on the acid digests prepared by 'wet ashing' and microwave extraction. Sixteen elements (As, Ba, Be, Cd, Co, Cr, Cu, Ga, Mn, Mo, Ni, pH, Sb, Se, V and Zn) were quantified, in the samples before extraction, in the extracts and in the residues. Concentrations of trace elements in the original biomass samples were lower than in the coal sample while the concentrations in the ash sample were the highest. The major trace elements in the NMP extracts were Ba, Cu, Mn and Zn from the forest residue; Ba, Cu, Mn, Pb and Zn from the coal; Cu and Zn from the ash. These elements are believed to be associated with the organic extracts from the forest residue and coal, and also from the ash.

  16. Determination of omeprazole and its metabolites in human plasma by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Kanazawa, Hideko; Okada, Akiko; Matsushima, Yoshikazu; Yokota, Hiromitsu; Okubo, Shigeo; Mashige, Fumiko; Nakahara, Kazuhiko

    2002-03-08

    Omeprazole is a benzimidazole compound that acts as a proton-pump inhibitor. Because the metabolism of omeprazole is mainly catalyzed by cytochrome P-450 (CYP) 3A4 and CYP2C19. the genetic polymorphism of CYP2C19 could be of clinical concern in the treatment of acid-related diseases with omeprazole. Therefore, a reliable method for omeprazole phenotyping is desirable in clinical situations. This study has demonstrated the determination of omeprazole and its metabolites in human plasma by liquid chromatography-three-dimensional quadrupole mass spectrometry with a sonic spray ionization interface. The analytical column was YMC-Pack Pro C18(50x2.0 mm I.D.) using acetonitrile-50 mM ammonium acetate (pH 7.25) (1:4) at a flow-rate of 0.2 ml/min. The drift voltage was 30 V. The sampling aperture was heated at 110 degrees C and Shield temperature was 230 degrees C. In the mass spectrum, the molecular ions of omeprazole, hydroxyomeprazole and omeprazole sulfone were clearly observed as base peaks. This method is sufficiently sensitive and accurate for pharmacokinetic studies of omeprazol.

  17. Separation Of Uranium And Plutonium Isotopes For Measurement By Multi Collector Inductively Coupled Plasma Mass Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Martinelli, R E; Hamilton, T F; Williams, R W; Kehl, S R

    2009-03-29

    Uranium (U) and plutonium (Pu) isotopes in coral soils, contaminated by nuclear weapons testing in the northern Marshall Islands, were isolated by ion-exchange chromatography and analyzed by mass spectrometry. The soil samples were spiked with {sup 233}U and {sup 242}Pu tracers, dissolved in minerals acids, and U and Pu isotopes isolated and purified on commercially available ion-exchange columns. The ion-exchange technique employed a TEVA{reg_sign} column coupled to a UTEVA{reg_sign} column. U and Pu isotope fractions were then further isolated using separate elution schemes, and the purified fractions containing U and Pu isotopes analyzed sequentially using multi-collector inductively coupled plasma mass spectrometer (MCICP-MS). High precision measurements of {sup 234}U/{sup 235}U, {sup 238}U/{sup 235}U, {sup 236}U/{sup 235}U, and {sup 240}Pu/{sup 239}Pu in soil samples were attained using the described methodology and instrumentation, and provide a basis for conducting more detailed assessments of the behavior and transfer of uranium and plutonium in the environment.

  18. Authenticity of Benin metalworks evaluated by inductively coupled plasma mass spectrometry and lead isotope analyses

    Science.gov (United States)

    Fabbri, E.; Soffritti, C.; Merlin, M.; Vaccaro, C.; Garagnani, G. L.

    2017-05-01

    Two metal plaques and a cock statuette belonging to a private collection and stylistically consistent with the Royal Art of Benin (Nigeria) were investigated in order to verify their authenticity. The characterization of alloys and patinas were carried out by inductively coupled plasma mass spectrometry, optical microscopy, scanning electron microscopy and energy dispersion spectroscopy, and X-Ray diffraction spectrometry. Furthermore, thermal ionization mass spectrometry was used to assess the abundances of lead isotopes and to attempt a dating by the measurement of 210Pb/204Pb ratio. The results showed that all three artefacts were mainly composed of low lead-brass alloys, with relatively high concentrations of zinc, antimony, cadmium and aluminum in the solid copper solution. Microstructures were mostly dendritic, typical of as-cast brasses, and characterized by recrystallized non-homogeneous twinned grains in areas corresponding to surface decorations, probably due to multiple hammering steps followed by partial annealing treatments. The matrix was composed of a cored α-Cu solid solution together with non-metallic inclusions, lead globules and Sn-rich precipitates in interdendritic spaces. On the surface of all metalworks, both copper and zinc oxides, a non-continuous layer of sulphur-containing contaminants and chloride-containing compounds, were identified. The lead isotope results were consistent with brasses produced shortly before or after 1900 CE. Overall, the data obtained by different techniques supported the hypothesis that the three artefacts were not authentic.

  19. Studies of selenium and xenon in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bricker, T.

    1994-07-27

    Since its development, inductively coupled plasma mass spectrometry (ICP-MS) has been a widely used analytical technique. ICP-MS offers low detection limits, easy determination of isotope ratios, and simple mass spectra from analyte elements. ICP-MS has been successfully employed for many applications including geological, environmental, biological, metallurgical, food, medical, and industrial. One specific application important to many areas of study involves elemental speciation by using ICP-MS as an element specific detector interfaced to liquid chromatography. Elemental speciation information is important and cannot be obtained by atomic spectrometric methods alone which measure only the total concentration of the element present. Part 1 of this study describes the speciation of selenium in human serum by size exclusion chromatography (SEC) and detection by ICP-MS. Although ICP-MS has been widely sued, room for improvement still exists. Difficulties in ICP-MS include noise in the background, matrix effects, clogging of the sampling orifice with deposited solids, and spectral interference caused by polyatomic ions. Previous work has shown that the addition of xenon into the central channel of the ICP decreases polyatomic ion levels. In Part 2 of this work, a fundamental study involving the measurement of the excitation temperature is carried out to further understand xenon`s role in the reduction of polyatomic ions. 155 refs.

  20. Sulfur-based absolute quantification of proteins using isotope dilution inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Lee, Hyun-Seok; Heun Kim, Sook; Jeong, Ji-Seon; Lee, Yong-Moon; Yim, Yong-Hyeon

    2015-10-01

    An element-based reductive approach provides an effective means of realizing International System of Units (SI) traceability for high-purity biological standards. Here, we develop an absolute protein quantification method using double isotope dilution (ID) inductively coupled plasma mass spectrometry (ICP-MS) combined with microwave-assisted acid digestion for the first time. We validated the method and applied it to certify the candidate protein certified reference material (CRM) of human growth hormone (hGH). The concentration of hGH was determined by analysing the total amount of sulfur in hGH. Next, the size-exclusion chromatography method was used with ICP-MS to characterize and quantify sulfur-containing impurities. By subtracting the contribution of sulfur-containing impurities from the total sulfur content in the hGH CRM, we obtained a SI-traceable certification value. The quantification result obtained with the present method based on sulfur analysis was in excellent agreement with the result determined via a well-established protein quantification method based on amino acid analysis using conventional acid hydrolysis combined with an ID liquid chromatography-tandem mass spectrometry. The element-based protein quantification method developed here can be generally used for SI-traceable absolute quantification of proteins, especially pure-protein standards.

  1. Isotope ratio analysis of individual sub-micrometer plutonium particles with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Esaka, Fumitaka; Magara, Masaaki; Suzuki, Daisuke; Miyamoto, Yutaka; Lee, Chi-Gyu; Kimura, Takaumi

    2010-12-15

    Information on plutonium isotope ratios in individual particles is of great importance for nuclear safeguards, nuclear forensics and so on. Although secondary ion mass spectrometry (SIMS) is successfully utilized for the analysis of individual uranium particles, the isobaric interference of americium-241 to plutonium-241 makes difficult to obtain accurate isotope ratios in individual plutonium particles. In the present work, an analytical technique by a combination of chemical separation and inductively coupled plasma mass spectrometry (ICP-MS) is developed and applied to isotope ratio analysis of individual sub-micrometer plutonium particles. The ICP-MS results for individual plutonium particles prepared from a standard reference material (NBL SRM-947) indicate that the use of a desolvation system for sample introduction improves the precision of isotope ratios. In addition, the accuracy of the (241)Pu/(239)Pu isotope ratio is much improved, owing to the chemical separation of plutonium and americium. In conclusion, the performance of the proposed ICP-MS technique is sufficient for the analysis of individual plutonium particles.

  2. Liquid chromatography-tandem mass spectrometric assay for the PARP inhibitor rucaparib in plasma.

    Science.gov (United States)

    Sparidans, Rolf W; Durmus, Selvi; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H

    2014-01-01

    A quantitative bioanalytical liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay for the poly(ADP-ribose) polymerase-1 inhibitor rucaparib was developed and validated. Plasma samples were pre-treated using protein precipitation with acetonitrile containing gefitinib as internal standard. Diluted extract was directly injected into the reversed-phase chromatographic system. The eluate was transferred into the electrospray interface with positive ionization and the analyte was detected in the selected reaction monitoring mode of a triple quadrupole mass spectrometer. The assay was validated in a 1.25-2000ng/ml calibration range with r(2)=0.9958±0.0012 for linear regression with quadratic weighting (n=6). Within day precisions (n=18) were 2.0-5.4%, between day (3 days; n=18) precisions 3.2-8.0% and accuracies (n=18) were 89.7-93.2%. At the lower limit of quantification (1.25ng/ml) these parameters were 9.6%, 13.7% and 85.3%, respectively. The drug was sufficiently stable under all relevant analytical conditions. Finally, the assay was successfully used to determine drug pharmacokinetics in female FVB wild type mice. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. A New Liquid Chromatography-Tandem Mass Spectrometry Method for Determination of Bisoprolol in Human Plasma Samples

    OpenAIRE

    Gabriela Peste; Nela Bibire; Mihai Apostu; Aurel Vlase; Corneliu Oniscu

    2009-01-01

    Liquid chromatography (LC) coupled with mass spectrometry (MS) detection is one of the most powerful analytical tools for organic compound analysis. The advantages of using LC/MS methods over HPLC methods include: selectivity, chromatographic integrity, peak assignment, structural information, and rapid method development. In this paper, a new liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the determination of bisoprolol in human plasma s...

  4. The Human Plasma Proteome Draft of 2017: Building on the Human Plasma PeptideAtlas from Mass Spectrometry and Complementary Assays.

    Science.gov (United States)

    Schwenk, Jochen M; Omenn, Gilbert S; Sun, Zhi; Campbell, David S; Baker, Mark S; Overall, Christopher M; Aebersold, Ruedi; Moritz, Robert L; Deutsch, Eric W

    2017-09-22

    Human blood plasma provides a highly accessible window to the proteome of any individual in health and disease. Since its inception in 2002, the Human Proteome Organization's Human Plasma Proteome Project (HPPP) has been promoting advances in the study and understanding of the full protein complement of human plasma and on determining the abundance and modifications of its components. In 2017, we review the history of the HPPP and the advances of human plasma proteomics in general, including several recent achievements. We then present the latest 2017-04 build of Human Plasma PeptideAtlas, which yields ~43 million peptide-spectrum matches and 122,730 distinct peptide sequences from 178 individual experiments at a 1% protein-level FDR globally across all experiments. Applying the latest Human Proteome Project Data Interpretation Guidelines, we catalog 3509 proteins that have at least two non-nested uniquely-mapping peptides of 9 amino acids or more and >1300 additional proteins with ambiguous evidence. We apply the same two-peptide guideline to historical PeptideAtlas builds going back to 2006 and examine the progress made in the past ten years in plasma proteome coverage. We also compare the distribution of proteins in historical PeptideAtlas builds in various RNA-abundance and cellular localization categories. We then discuss advances in plasma proteomics based on targeted mass spectrometry as well as affinity assays, which during early 2017 target ~2000 proteins. Finally we describe considerations about sample handling and study design, concluding with an outlook for future advances in deciphering the human plasma proteome.

  5. Immunodepletion Plasma Proteomics by TripleTOF 5600 and Orbitrap Elite/LTQ-Orbitrap Velos/Q Exactive Mass Spectrometers

    Science.gov (United States)

    Patel, Bhavinkumar B.; Kelsen, Steven G.; Braverman, Alan; Swinton, Derrick J.; Gafken, Philip R.; Jones, Lisa A.; Lane, William S.; Neveu, John M.; Leung, Hon-Chiu E.; Shaffer, Scott A.; Leszyk, John D.; Stanley, Bruce A.; Fox, Todd E.; Stanley, Anne; Hall, Michael J.; Hampel, Heather; South, Christopher D.; de la Chapelle, Albert; Burt, Randall W.; Jones, David A.; Kopelovich, Levy; Yeung, Anthony T.

    2013-01-01

    Plasma proteomic experiments performed rapidly and economically using several of the latest high-resolution mass spectrometers were compared. Four quantitative hyperfractionated plasma proteomics experiments were analyzed in replicates by two AB SCIEX TripleTOF 5600 and three Thermo Scientific Orbitrap (Elite/LTQ-Orbitrap Velos/Q Exactive) instruments. Each experiment compared two iTRAQ isobaric-labeled immunodepleted plasma proteomes, provided as 30 labeled peptide fractions. 480 LC-MS/MS runs delivered >250 GB of data in two months. Several analysis algorithms were compared. At 1 % false discovery rate, the relative comparative findings concluded that the Thermo Scientific Q Exactive Mass Spectrometer resulted in the highest number of identified proteins and unique sequences with iTRAQ quantitation. The confidence of iTRAQ fold-change for each protein is dependent on the overall ion statistics (Mascot Protein Score) attainable by each instrument. The benchmarking also suggested how to further improve the mass spectrometry parameters and HPLC conditions. Our findings highlight the special challenges presented by the low abundance peptide ions of iTRAQ plasma proteome because the dynamic range of plasma protein abundance is uniquely high compared with cell lysates, necessitating high instrument sensitivity. PMID:24004147

  6. Fast quantification of endogenous carbohydrates in plasma using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Zhu, Bangjie; Liu, Feng; Li, Xituo; Wang, Yan; Gu, Xue; Dai, Jieyu; Wang, Guiming; Cheng, Yu; Yan, Chao

    2015-01-01

    Endogenous carbohydrates in biosamples are frequently highlighted as the most differential metabolites in many metabolomics studies. A simple, fast, simultaneous quantitative method for 16 endogenous carbohydrates in plasma has been developed using hydrophilic interaction liquid chromatography coupled with tandem mass spectrometry. In order to quantify 16 endogenous carbohydrates in plasma, various conditions, including columns, chromatographic conditions, mass spectrometry conditions, and plasma preparation methods, were investigated. Different conditions in this quantified analysis were performed and optimized. The reproducibility, precision, recovery, matrix effect, and stability of the method were verified. The results indicated that a methanol/acetonitrile (50:50, v/v) mixture could effectively and reproducibly precipitate rat plasma proteins. Cold organic solvents coupled with vortex for 1 min and incubated at -20°C for 20 min were the most optimal conditions for protein precipitation and extraction. The results, according to the linearity, recovery, precision, matrix effect, and stability, showed that the method was satisfactory in the quantification of endogenous carbohydrates in rat plasma. The quantified analysis of endogenous carbohydrates in rat plasma performed excellently in terms of sensitivity, high throughput, and simple sample preparation, which met the requirement of quantification in specific expanded metabolomic studies after the global metabolic profiling research.

  7. Applications of ICP magnetic sector multicollector mass spectrometry to basic energy research. Final report for period December 1st, 1993 - May 31st, 2000

    Energy Technology Data Exchange (ETDEWEB)

    Halliday, A.N.

    2002-05-01

    The primary aims of this research were threefold: to develop and utilize the new technique of multiple collector inductively coupled plasma mass spectrometry and apply it to problems in the earth, ocean, and environmental sciences; to develop new chronometers and improve existing chronometers to allow the accurate determination of the ages of geological features and processes; and to study natural fluid-mediated mass transfer processes and source of components in the crust and the oceans. This technique has now become the preferred method for the determination of the isotopic compositions of a variety of elements in the periodic table. The prototype instrument was used to explore a vast array of isotopic systems and demonstrate applicability to problems as different as the origin of the solar system and smelting methods in the Bronze Age. Highlights of the program are briefly summarized under the following topics: tungsten isotopes and the early solar system; trace siderophile and chalcophile element geochemistry; hafnium isotopes and the early development of the continents; evolution of lead isotopic compositions of the oceans; the isotopic composition and residence time of Hf in seawater; the isotopic compositions of Sr, Hf, Pb, and Nd in dust; U-Th disequilibrium dating of carbonates and soils; in situ U-Th disequilibrium dating of opal.

  8. Determination of platinum surface contamination in veterinary and human oncology centres using inductively coupled plasma mass spectrometry

    NARCIS (Netherlands)

    Janssens, T.; Brouwers, E. E M; de Vos, J. P.; de Vries, N.; Schellens, J. H M; Beijnen, J. H.

    2015-01-01

    The objective of this study was to determine the surface contamination with platinum-containing antineoplastic drugs in veterinary and human oncology centres. Inductively coupled plasma mass spectrometry was used to measure platinum levels in surface samples. In veterinary and human oncology

  9. Quantitation of isobaric phosphatidylcholine species in human plasma using a hybrid quadrupole linear ion trap mass spectrometer

    Science.gov (United States)

    Phosphatidylcholine (PC) species in human plasma are used as biomarkers of disease. PC biomarkers are often limited by the inability to separate isobaric PC. In this work, we developed a targeted shotgun approach for analysis of isobaric and isomeric PC. This approach is comprised of two mass spectr...

  10. Determination of selenite and selenate in human urine by ion chromatography and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.

    2000-01-01

    monitored in the inductively coupled plasma mass spectrometry (ICP-MS) detector. When the chromatographic system was applied to analysis of urine samples diluted 1 + 1, the selenomethionine signal appeared in the front together with other unresolved selenium species, while the selenite and selenate signals...

  11. Characterization of isomeric VX nerve agent adducts on albumin in human plasma using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Saeidian, Hamid; Mirkhani, Valioallah; Mousavi Faraz, Sajjad; Taghi Naseri, Mohammad; Babri, Mehran

    2015-01-01

    This study includes the characterization of isomeric VX organophosphorus adducts on albumin in human plasma using liquid chromatography-tandem mass spectrometry (LC-MS/MS). VX or its structural isomers were spiked into a vial containing plasma in order to obtain phosphorylated albumin. After pronase and trypsin digestion, the resulting solutions were analyzed to confirm adduct formation with the amino acid tyrosine on the albumin in human plasma. The LC-MS/MS experiments show that VX and its isomers can be attached to tyrosine on the albumin in human blood. Mass spectrometric studies revealed some interesting fragmentation pathways during the ionization process, such as ethylene, formic acid and ammonia elimination and an intermolecular electrophilic aromatic substitution reaction. The proposed mechanisms for the formation of the fragments were confirmed through the analysis of fragments of deuterated adducts.

  12. Momentum, Heat, and Neutral Mass Transport in Convective Atmospheric Pressure Plasma-Liquid Systems and Implications for Aqueous Targets

    CERN Document Server

    Lindsay, Alexander; Slikboer, Elmar; Shannon, Steven; Graves, David

    2015-01-01

    There is a growing interest in the study of plasma-liquid interactions with application to biomedicine, chemical disinfection, agriculture, and other fields. This work models the momentum, heat, and neutral species mass transfer between gas and aqueous phases in the context of a streamer discharge; the qualitative conclusions are generally applicable to plasma-liquid systems. The problem domain is discretized using the finite element method. The most interesting and relevant model result for application purposes is the steep gradients in reactive species at the interface. At the center of where the reactive gas stream impinges on the water surface, the aqueous concentrations of OH and ONOOH decrease by roughly 9 and 4 orders of magnitude respectively within 50 $\\mu$m of the interface. Recognizing the limited penetration of reactive plasma species into the aqueous phase is critical to discussions about the therapeutic mechanisms for direct plasma treatment of biological solutions. Other interesting results fro...

  13. Lowering plasma frequency by enhancing the effective mass of electrons: A route to deep sub-wavelength metamaterials

    Institute of Scientific and Technical Information of China (English)

    Qin Gang; Wang Jia-Fu; Yan Ming-Bao; Chen Wei; Chen Hong-Ya; Li Yong-Feng

    2013-01-01

    Deep sub-wavelength metamaterials are the key to the further development of practical metamaterials with small volumes and broadband properties.We propose to reduce the electrical sizes of metamaterials down to more sub-wavelength scales by lowering the plasma frequencies of metallic wires.The theoretical model is firstly established by analyzing the plasma frequency of continuous thin wires.By introducing more inductance elements,the effective electron mass can be enhanced drastically,leading to significantly lowered plasma frequencies.Based on this theory,we demonstrate that both the electric and the magnetic plasma frequencies of metamaterials can be lowered significantly and thus the electrical sizes of metamaterials can be reduced to more sub-wavelength scales.This provides an efficient route to deep sub-wavelength metamaterials and will give rigorous impetus for the further development of practical metamaterials.

  14. Dilepton production as a useful probe of quark gluon plasma with temperature dependent chemical potential quark mass

    Science.gov (United States)

    Kumar, Yogesh; Singh, S. Somorendro

    2016-07-01

    We extend the previous study of dilepton production using [S. Somorendro Singh and Y. Kumar, Can. J. Phys. 92 (2014) 31] based on a simple quasiparticle model of quark-gluon plasma (QGP). In this model, finite value of quark mass uses temperature dependent chemical potential the so-called Temperature Dependent Chemical Potential Quark Mass (TDCPQM). We calculate dilepton production in the relevant range of mass region. It is observed that the production rate is marginally enhanced from the earlier work. This is due to the effect of TDCPQM and its effect is highly significant in the production of dilepton.

  15. Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

    Science.gov (United States)

    Wolf, Ruth E.; Adams, Monique

    2015-01-01

    Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

  16. Confirmatory analysis of acetylgestagens in plasma using liquid chromatography-tandem mass spectrometry

    DEFF Research Database (Denmark)

    Mortensen, Sarah Kelly; Pedersen, Mikael

    2007-01-01

    A confirmatory method has been developed and validated for the determination of chlormadinone acetate (CMA), megestrol acetate (NIGA), melengestrol acetate (MLA) and medroxyprogesterone acetate (MPA) in bovine and porcine plasma. Analytes are extracted from plasma samples using matrix-assisted li......A confirmatory method has been developed and validated for the determination of chlormadinone acetate (CMA), megestrol acetate (NIGA), melengestrol acetate (MLA) and medroxyprogesterone acetate (MPA) in bovine and porcine plasma. Analytes are extracted from plasma samples using matrix...

  17. Characterization of microconcentric nebulizer uptake rates for capillary electrophoresis inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Yanes, Enrique G.; Miller-Ihli, Nancy J.

    2003-05-01

    There is demonstrated interest in combining capillary electrophoresis (CE) with inductively coupled plasma mass spectrometry (ICP-MS) for speciation determinations. When self-aspirating nebulizers are used for this application, it is important to offset the suction effect to avoid degradation of the separation. In this study, sample uptake rates for three microconcentric nebulizers of the same model, in combination with a cyclonic spray chamber, were characterized and compared for future utilization in CE-ICP-MS interfaces. The specific model studied was a MicroMist with a nominal uptake rate of 100 μl/min at 1 l/min argon gas flow rate per the manufacturer's specifications. Sample uptake rates at various nebulizer gas flows were measured by aspirating water from a weighed container and calculating the uptake rate in microliter per minute. The nebulizers studied provided good reproducibility from day to day, but a comparison of the different nebulizers reflected a significant difference in performance. A characteristic observed during the study was that uptake rates decreased with increasing nebulizer gas flow. This can be used for sample introduction for CE-ICP-MS. Interestingly, very different performance was observed when comparing the three different nebulizers of the same model. Uptake rates showed strong dependence on argon gas flow rates and the dimensions of the sample uptake tubing.

  18. Accurate determination of silver nanoparticles in animal tissues by inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Veverková, Lenka [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Hradilová, Šárka [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Milde, David, E-mail: david.mlde@upol.cz [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Panáček, Aleš [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Skopalová, Jana [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Kvítek, Libor [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Petrželová, Kamila [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); National Reference Laboratory for Chemical Elements, Department of Residues in Kroměříž, State Veterinary Institute Olomouc, Hulínská 2286, CZ 767 60 Kroměříž (Czech Republic); and others

    2014-12-01

    This study examined recoveries of silver determination in animal tissues after wet digestion by inductively coupled plasma mass spectrometry. The composition of the mineralization mixture for microwave assisted digestion was optimized and the best recoveries were obtained for mineralization with HNO{sub 3} and addition of HCl promptly after digestion. The optimization was performed on model samples of chicken meat spiked with silver nanoparticles and a solution of ionic silver. Basic calculations of theoretical distribution of Ag among various silver-containing species were implemented and the results showed that most of the silver is in the form of soluble complexes AgCl{sub 2}{sup −} and AgCl{sub 3}{sup 2−} for the optimized composition of the mineralization mixture. Three animal tissue certified reference materials were then analyzed to verify the trueness and precision of the results. - Highlights: • We performed detailed optimization of microwave assisted digestion procedure of animal tissue used prior to Ag determination by ICP-MS. • We provide basic equilibrium calculations to give theoretical explanation of results from optimization of tested mineralization mixtures. • Results from method validation that was done by analysis of several matrix CRMs are presented.

  19. Determination of Menthol in Plasma and Urine by Gas Chromatography/Mass Spectrometry (GC/MS).

    Science.gov (United States)

    Peat, Judy; Frazee, Clint; Kearns, Gregory; Garg, Uttam

    2016-01-01

    Menthol, a monoterpene, is a principal component of peppermint oil and is used extensively in consumer products as a flavoring aid. It is also commonly used medicinally as a topical skin coolant; to treat inflammation of the mucous membranes, digestive problems, and irritable bowel syndrome (IBS); and in preventing spasms during endoscopy and for its spasmolytic effect on the smooth muscle of the gastrointestinal tract. Menthol has a half life of 3-6 h and is rapidly metabolized to menthol glucuronide which is detectable in urine and serum following menthol use. We describe a method for the determination of total menthol in human plasma and urine using liquid/liquid extraction, gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring mode and menthol-d4 as the internal standard. Controls are prepared with menthol glucuronide and all samples undergo enzymatic hydrolysis for the quantification of total menthol. The method has a linear range of 5-1000 ng/mL, and coefficient of variation <10%.

  20. Determination of impurity elements in MnZn ferrites by inductively coupled plasma mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    张萍; 符靓; 马俊才; 唐有根

    2015-01-01

    An inductively coupled plasma mass spectrometry (ICP-MS) method was developed for the determination of Na, Mg, Al, K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+HCl with microwave digestion followed by dilution with ultrapure water, then the above 16 impurity elements in the solution were analyzed directly by ICP-MS. The impurity elements were introduced by the helium gas or hydrogen gas into the octopole reaction system (ORS) to eliminate the polyatomic interferences caused by the high salty matrixes. The matrix effect was minimized through matrix matching, and Be, Y and Rh were used as internal standard elements. The working parameters of the instrument were optimized. The results show that the method has good precision and high accuracy. The detection limits for the investigated elements are in the range of 0.9−37.5 ng/L, the relative standard deviation of each element is within 1.1%−4.8%, and the recovery of each element is 90%−108%.

  1. Determination of stable cesium and strontium in rice samples by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Srinuttrakul, W.; Yoshida, S.

    2017-06-01

    For long-term radiation dose assessment models, food ingestion is one of the major exposure pathways to human. In general, the stable isotopes can serve as analogues of radioisotopes. In this study, rice samples were collected from 30 paddy fields in Si Sa Ket, Yasothon and Roi Et in the northeast of Thailand in November 2014. The concentrations of stable cesium (Cs-133) and strontium (Sr-88) in polished rice were determined by inductively coupled plasma mass spectrometry (ICP-MS). The standard reference material of rice flour (NIST 1568a) with spiked Cs and Sr was used to validate the analytical method. The concentration of Cs in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.158 ± 0.167 mg kg-1, 0.090 ± 0.117 mg kg-1 and 0.054 ± 0.031 mg kg-1, respectively. The concentration of Sr in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.351 ± 0.108 mg kg-1, 0.364 ± 0.215 mg kg-1 and 0.287 ± 0.102 mg kg-1, respectively. Comparison of the results with Japanese data before the Fukushima Di-ichi nuclear power plant accident showed that the concentrations of both Cs and Sr for Thai rice were higher than those for Japanese rice.

  2. Comparison of femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry for uranium isotopic measurements

    Energy Technology Data Exchange (ETDEWEB)

    Havrilla, George Joseph [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); McIntosh, Kathryn Gallagher [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Judge, Elizabeth [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Dirmyer, Matthew R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Campbell, Keri [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Gonzalez, Jhanis J. [Applied Spectra Inc., Fremont, CA (United States)

    2016-10-20

    Feasibility tests were conducted using femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry for rapid uranium isotopic measurements. The samples used in this study consisted of a range of pg quantities of known 235/238 U solutions as dried spot residues of 300 pL drops on silicon substrates. The samples spanned the following enrichments of 235U: 0.5, 1.5, 2, 3, and 15.1%. In this direct comparison using these particular samples both pulse durations demonstrated near equivalent data can be produced on either system with respect to accuracy and precision. There is no question that either LA-ICP-MS method offers the potential for rapid, accurate and precise isotopic measurements of U10Mo materials whether DU, LEU or HEU. The LA-ICP-MS equipment used for this work is commercially available. The program is in the process of validating this work for large samples using center samples strips from Y-12 MP-1 LEU-Mo Casting #1.

  3. Profiling metals in Cordyceps sinensis by using inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Wei, Xin; Hu, Hankun; Zheng, Baogeng; Arslan, Zikri; Huang, Hung-Chung; Mao, Weidong; Liu, Yi-Ming

    2017-01-28

    Cordyceps sinensis (C. sinensis) is a natural product that has diverse nutritional and medicinal values. Since the availability of natural C. sinensis becomes limited its authentication and quality control is of high significance. Herein we report on profiling of metals in C. sinensis by using inductively coupled plasma mass spectrometry (ICP-MS). The analysis reveals that C. sinensis contains a wide array of essential elements, including P, Mg, Zn, Cu, Fe, etc. Toxic metals detected are Cd, Pb, and As. In all five samples analyzed Pb contents are below 2.0 ppm. Arsenic level in C. sinensis caterpillar is significantly higher than that in its mycelium and varies from 3.0 to 32 ppm likely due to soil contamination. It's for the first time demonstrated in this work that clustering analysis on the proposed metal profiles consisting of 24 elements is very useful to identify "abnormal" C. sinensis samples, thus adding another dimension to the effective means for authentication and quality assessment of this highly demanded previous natural product.

  4. Fundamental and methodological investigations for the improvement of elemental analysis by inductively coupled plasma mass soectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ebert, Christopher Hysjulien [Ames Lab., Ames, IA (United States)

    2012-01-01

    This dissertation describes a variety of studies meant to improve the analytical performance of inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation (LA) ICP-MS. The emission behavior of individual droplets and LA generated particles in an ICP is studied using a high-speed, high frame rate digital camera. Phenomena are observed during the ablation of silicate glass that would cause elemental fractionation during analysis by ICP-MS. Preliminary work for ICP torch developments specifically tailored for the improvement of LA sample introduction are presented. An abnormal scarcity of metal-argon polyatomic ions (MAr{sup +}) is observed during ICP-MS analysis. Evidence shows that MAr{sup +} ions are dissociated by collisions with background gas in a shockwave near the tip of the skimmer cone. Method development towards the improvement of LA-ICP-MS for environmental monitoring is described. A method is developed to trap small particles in a collodion matrix and analyze each particle individually by LA-ICP-MS.

  5. Determination of cobalamins using capillary electrophoresis inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Baker, S. A.; Miller-Ihli, N. J.

    2000-12-01

    The determination of cobalamins using capillary electrophoresis inductively coupled plasma mass spectrometry (CE-ICP-MS) was investigated. Both capillary zone electrophoresis (CZE) and micellar electrokinetic chromatography (MEKC) modes of operation were studied. The optimal separation of four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) and a potentially harmful corrinoid analogue (cobinamide dicyanide) was obtained using CZE at a pH of 2.5. Both 20 mM phosphate and 20 mM formate buffers were used with success, although the formate buffer provided improved resolution. The CZE-ICP-MS method was used to quantify cyanocobalamin in a vitamin supplement and the analytical results were in good agreement (±5%) with values obtained by ICP-MS for total Co levels. The solution detection limits for cobalamins using CZE-ICP-MS were approximately 50 ng/ml. MEKC was found to be useful for the screening of vitamin preparations because it provided a rapid means of distinguishing cyanocobalamin (the form most commonly used in vitamin preparations) from free cobalt. The separation of free cobalt and cyanocobalamin using MEKC was achieved in less than 10 min.

  6. Thin-layer chromatography combined with diode laser thermal vaporization inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Bednařík, Antonín; Tomalová, Iva; Kanický, Viktor; Preisler, Jan

    2014-10-17

    Here we present a novel coupling of thin-layer chromatography (TLC) to diode laser thermal vaporization inductively coupled plasma mass spectrometry (DLTV ICP MS). DLTV is a new technique of aerosol generation which uses a diode laser to induce pyrolysis of a substrate. In this case the cellulose stationary phase on aluminum-backed TLC sheets overprinted with black ink to absorb laser light. The experimental arrangement relies on economic instrumentation: an 808-nm 1.2-W continuous-wave infrared diode laser attached to a syringe pump serving as the movable stage. Using a glass tubular cell, the entire length of a TLC separation channel is scanned. The 8-cm long lanes were scanned in ∼35 s. The TLC - DLTV ICP MS coupling is demonstrated on the separation of four cobalamins (hydroxo-; adenosyl-; cyano-; and methylcobalamin) with limits of detection ∼2 pg and repeatability ∼15% for each individual species. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Establishing human heart chromium, cobalt and vanadium concentrations by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Day, Patrick L; Eckdahl, Steven J; Maleszewski, Joseph J; Wright, Thomas C; Murray, David L

    2017-05-01

    Chromium, cobalt, and vanadium are used in metallic joint prosthesis. Case studies have associated elevated heart tissue cobalt concentrations with myocardial injury. To document the long term heart metal ion concentrations, a validated inductively coupled plasma mass spectroscopy (ICP-MS) method was needed. The method utilized a closed-vessel microwave digestion system to digest the samples. An ICP-MS method utilizing Universal Cell Technology was used to determine our target analyte concentrations. Accuracy was verified using reference materials. Precision, sensitivity, recovery and linearity studies were performed. This method was used to establish a reference range for a non-implant containing cohort of 80 autopsy human heart tissues RESULTS: This method demonstrated an analytic measurement range of 0.5-100ng/mL for each element. Accuracy was within ±10% of target value for each element. Within-run precision for each element was below 20% CV. The chromium, vanadium and cobalt concentrations (mean±SD) were 0.1523±0.2157μg/g, 0.0094±0.0211μg/g and 0.1039±0.1305μg/g respectively in 80 non-implant containing human heart tissue samples. This method provides acceptable recovery of the chromium, cobalt and vanadium in heart tissue; allowing assessment of the effects of metallic joint prosthesis on myocardial health. Copyright © 2017 Elsevier GmbH. All rights reserved.

  8. Trace Elements Analysis of Geological Samples by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    This paper describes recent work applying a taser ablation system (LSX-200) hyphenated with POEMS Ⅲ inductively coupled plasma mass spectrometry (LA-ICP-MS) for the in situ analysis of 22 trace elements of solid geological materials. It demonstrates the potential of LA-ICP-MS for the determination of geochemically important trace and ultra-trace elements following XRF routine sample preparation. Signal drift, difference in transport efficiency and sampling yield are well corrected with NIST SRM 612 as external calibration standard and Ca as internal standard. The obtained results agree to the recommended values with relative error better than 15 % and RSD less than 15 % for most determined trace elemems. LOD ranges from 0.021 × 10-6 to 0. 23 × 10-6 and less than 0.10 × 10-6 for majority trace elements determined. In addition, home-made macro functions including filter and calculator compiled by VBA language under Excel software greatly enhanced off-line data reduction efficiency.``

  9. Inductively coupled plasma mass spectrometer with laser ablation metal ions release detection in the human mouth

    Science.gov (United States)

    Kueerova, Hana; Dostalova, Tatjana; Prochazkova, J.

    2002-06-01

    Presence of more dental alloys in oral cavity often causes pathological symptoms. Due to various and multi-faced symptomatology, they tend to be a source of significant problems not only for the patient but also for the dentist. Metal ions released from alloys can cause subjective and objective symptoms in mouth. The aim of this study was detection of metal elements presence in saliva. There were 4 groups of examined persons: with intact teeth (15 individuals) with metallic restorations, pathological currents 5-30 (mu) A, multi-faced subjective symptomatology and uncharacteristic objective diagnosis (32 patients), with metallic restorations and no subjective symptoms (14 persons) and with metallic restorations, without pathological currents and with problems related to galvanism (13 patients). Presence of 14 metal elements was checked by inductively coupled plasma mass spectrometer with laser ablation. Nd:YAG laser detector was used. There were significant differences in content of silver, gold and mercury between persons with intact teeth and other three groups. There were no differences found between subjects with and without galvanic currents, and presence of subjective and objective symptoms.

  10. Laser ablation - inductively coupled plasma mass spectrometry (LA-ICP-MS): Novel applications for coal research

    Energy Technology Data Exchange (ETDEWEB)

    Booth, C.A.; Spears, D.A.

    1999-07-01

    Laser Ablation - Inductively Coupled Plasma - Mass Spectrometry (LA-ICP-MS) has enormous potential in coal research. Element concentrations are determined with limits of detection currently in the parts per billion range, whilst spatial resolution as low as 10 microns can be achieved using the CETAC Technologies LSX-100 laser ablation system. Calibration of the LA-ICP-MS systems is notoriously difficult but in this paper the authors review two different techniques used in Sheffield, which allow trace element concentrations of whole coals (bituminous) and minerals and macerals within the coal to be determined. The first technique involves calibrating the system with PF grade coal samples in order that trace element concentrations can directly be determined after ablation of a solid coal or pressed coal sample. Using this technique, potentially hazardous trace elements such as As, Cd, Pb and Hg can be detected and measured even in the low parts per billion concentration (mg/Kg) range. The second application utilizes the spatial resolution of the laser to measure element concentrations in individual coal components. In this paper the results from ablating pyrite framboids in polished sections of the coal are discussed. Elemental information is obtained throughout the ablation procedure and this is then calibrated against the Fe content in order to establish the concentration of an element per 1% pyritic iron.

  11. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J.M.; García Alonso, J.I., E-mail: jiga@uniovi.es

    2015-06-01

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC–ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review. - Highlights: • Emphasis placed on the sulfur-specific detection by chromatographic techniques coupled on-line to ICP-MS. • Different instrumental approaches available for sulfur measurements by ICP-MS. • Quantification of proteins and the analysis of metalloproteins via sulfur by LC-ICP-MS. • Labelling procedures for metabolic applications are also included. • The measurement of natural variations in S isotope composition with multicollector ICP-MS.

  12. Element fingerprinting of marine organisms by dynamic reaction cell inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Cubadda, Francesco; Raggi, Andrea; Coni, Ettore

    2006-02-01

    A method for the determination of sixteen elements (Al, As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Se, Sn, V, Zn) in seafood by dynamic reaction cell inductively coupled plasma mass spectrometry (ICP-DRC-MS) is presented. A preliminary study of polyatomic interferences was carried out in relation to the chemical composition of marine organisms belonging to different taxa. Acid effects and other matrix effects in marine organisms submitted to closed-vessel microwave digestion were investigated as well. Ammonia was the reactive gas used in the DRC to remove polyatomic ions interfering with 27Al, 52Cr, 56Fe and 51V. Optimal conditions for the simultaneous determination of analytes were identified in order to develop a fast multielement method. A suite of real samples (mussels and various fish species) were used during method development along with three certified reference materials: BCR CRM 278R (mussel tissue), BCR CRM 422 (cod muscle) and DORM-2 (dogfish muscle). The proposed analytical approach can be used in conjunction with suitable chemometric procedures to address quality and safety issues in aquaculture and fisheries. As an example, a case study is described in which mussels from three farming sites in the Venice Lagoon were distinguished by multivariate analysis of element fingerprints.

  13. Laser ablation inductively coupled plasma mass spectrometry imaging of metals in experimental and clinical Wilson's disease.

    Science.gov (United States)

    Boaru, Sorina Georgiana; Merle, Uta; Uerlings, Ricarda; Zimmermann, Astrid; Flechtenmacher, Christa; Willheim, Claudia; Eder, Elisabeth; Ferenci, Peter; Stremmel, Wolfgang; Weiskirchen, Ralf

    2015-04-01

    Wilson's disease is an autosomal recessive disorder in which the liver does not properly release copper into bile, resulting in prominent copper accumulation in various tissues. Affected patients suffer from hepatic disorders and severe neurological defects. Experimental studies in mutant mice in which the copper-transporting ATPase gene (Atp7b) is disrupted revealed a drastic, time-dependent accumulation of hepatic copper that is accompanied by formation of regenerative nodes resembling cirrhosis. Therefore, these mice represent an excellent exploratory model for Wilson's disease. However, the precise time course in hepatic copper accumulation and its impact on other trace metals within the liver is yet poorly understood. We have recently established novel laser ablation inductively coupled plasma mass spectrometry protocols allowing quantitative metal imaging in human and murine liver tissue with high sensitivity, spatial resolution, specificity and quantification ability. By use of these techniques, we here aimed to comparatively analyse hepatic metal content in wild-type and Atp7b deficient mice during ageing. We demonstrate that the age-dependent accumulation of hepatic copper is strictly associated with a simultaneous increase in iron and zinc, while the intrahepatic concentration and distribution of other metals or metalloids is not affected. The same findings were obtained in well-defined human liver samples that were obtained from patients suffering from Wilson's disease. We conclude that in Wilson's disease the imbalances of hepatic copper during ageing are closely correlated with alterations in intrahepatic iron and zinc content.

  14. Imaging gold nanoparticles in mouse liver by laser ablation inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Li, Qing; Wang, Zheng; Mo, Jiamei; Zhang, Guoxia; Chen, Yirui; Huang, Chuchu

    2017-06-07

    Imaging the size distribution of metal nanoparticles (NPs) in a tissue has important implications in terms of evaluating NP toxicity. Microscopy techniques used to image tissue NPs are limited by complicated sample preparation or poor resolution. In this study, we developed a laser ablation (LA) system coupled to single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) for quantitative imaging of gold (G)NPs in tissue samples. In this system, GNPs were ablated but did not disintegrate and integrate under optimised operation conditions, which were verified by characterising LA particles by scanning electron microscopy. The feasibility of imaging size distributions in tissue was validated using reference GNPs 60 and 80 nm in size on matrix-matched kidney. A transport efficiency of 6.07% was obtained by LA-SP-ICP-MS under optimal conditions. We used this system to image 80-nm GNPs in mouse liver and the size distribution thus obtained was in accordance with that determined by nebuliser SP-ICP-MS. The images revealed that 80-nm GNPs mainly accumulate in the liver and did not obviously aggregate. Our results demonstrate that LA-SP-ICP-MS is an effective tool for evaluating the size distribution of metal NPs in tissue.

  15. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Applications in Quantitative Proteomics.

    Science.gov (United States)

    Chahrour, Osama; Malone, John

    2017-01-01

    Recent advances in inductively coupled plasma mass spectrometry (ICP-MS) hyphenated to different separation techniques have promoted it as a valuable tool in protein/peptide quantification. These emerging ICP-MS applications allow absolute quantification by measuring specific elemental responses. One approach quantifies elements already present in the structure of the target peptide (e.g. phosphorus and sulphur) as natural tags. Quantification of these natural tags allows the elucidation of the degree of protein phosphorylation in addition to absolute protein quantification. A separate approach is based on utilising bi-functional labelling substances (those containing ICP-MS detectable elements), that form a covalent chemical bond with the protein thus creating analogs which are detectable by ICP-MS. Based on the previously established stoichiometries of the labelling reagents, quantification can be achieved. This technique is very useful for the design of precise multiplexed quantitation schemes to address the challenges of biomarker screening and discovery. This review discusses the capabilities and different strategies to implement ICP-MS in the field of quantitative proteomics. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  16. Inductively-coupled plasma mass spectrometry in proteomics, metabolomics and metallomics studies.

    Science.gov (United States)

    Mounicou, Sandra; Szpunar, Joanna; Lobinski, Ryszard

    2010-01-01

    The potential of inductively-coupled plasma mass spectrometry (ICP-MS) and its complementarity to soft- ionization MS techniques are discussed in the context of the analysis for biomolecules. ICP-MS offers detection limits in the attomolar range, regardless of the molecular environment of the target element. The sensitivity is hardly affected by the sample matrix, chromatographic mobile phase, or co-eluted compounds. The abundance sensitivity over six decades and the linear dynamic range over nine decades make simultaneous multi-isotopic analysis routinely possible. The manuscript discusses the state-of-the-art of ICP-MS for the detection of proteins in gel electrophoresis and of peptides in 2D high-performance liquid chromatography. The possibilities of quantification to the degree of some post-translational modifications are highlighted. Attention is also paid to the role of ICP-MS in protein quantification via metal-coded labeling and to the use of differentially-labeled antibodies for the multiplexed biomarker analysis. The key role of ICP-MS in the emerging area of metallomics is briefly discussed.

  17. Depleted uranium analysis in blood by inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Todorov, T.I.; Xu, H.; Ejnik, J.W.; Mullick, F.G.; Squibb, K.; McDiarmid, M.A.; Centeno, J.A.

    2009-01-01

    In this study we report depleted uranium (DU) analysis in whole blood samples. Internal exposure to DU causes increased uranium levels as well as change in the uranium isotopic composition in blood specimen. For identification of DU exposure we used the 235U/238U ratio in blood samples, which ranges from 0.00725 for natural uranium to 0.002 for depleted uranium. Uranium quantification and isotopic composition analysis were performed by inductively coupled plasma mass spectrometry. For method validation we used eight spiked blood samples with known uranium concentrations and isotopic composition. The detection limit for quantification was determined to be 4 ng L-1 uranium in whole blood. The data reproduced within 1-5% RSD and an accuracy of 1-4%. In order to achieve a 235U/238U ratio range of 0.00698-0.00752% with 99.7% confidence limit a minimum whole blood uranium concentration of 60 ng L??1 was required. An additional 10 samples from a cohort of veterans exposed to DU in Gulf War I were analyzed with no knowledge of their medical history. The measured 235U/ 238U ratios in the blood samples were used to identify the presence or absence of DU exposure within this patient group. ?? 2009 The Royal Society of Chemistry.

  18. Development of Localized Plasma Etching System for Failure Analyses in Semiconductor Devices: (3)Etching-Monitoring Using Quadrupole Mass Spectrometry

    Science.gov (United States)

    Takahashi, Satoshi; Horie, Tomoyuki; Shirayama, Yuya; Yokosuka, Shuntaro; Kashimura, Kenta; Hayashi, Akihiro; Iwase, Chikatsu; Shimbori, Shun'ichiro; Tokumoto, Hiroshi; Naitoh, Yasuhisa; Shimizu, Tetsuo

    Quadrupole mass spectrometry (QMS) has been applied to monitor the etching processes in a localized plasma etching system. An inward plasma was employed for etching in which the etching gas was discharged in the narrow gap between the etched sample and the entrance of an evacuating capillary tube. As the etching products are immediately evacuated through the capillary, a QMS system equipped at the capillary exit is able to analyze the products without any loss in concentration via diffusion into the chamber. Two kinds of samples, thermally grown SiO2 on Si and spin-coated polyimide film on Si, were etched, and the chemical species in the evacuated etching gas were analyzed with QMS, which enables monitoring of the composition of the surface being etched. Samples of thermal SiO2 were etched with CF4 plasma. The peak height of the SiF3+ signal during the SiO2 etching was lower than that observed during etching of the silicon substrate, leading to endpoint detection. The endpoint detection of the polyimide film etching was conducted using two etching gases: pure O2 and pure CF4. When O2 was used, the endpoint was detected by the decrease of the mass peak attributed to CO. When CF4 was employed, the plasma was able to etch both the polyimide film and Si substrate. Then the endpoint was detected by the increase of the mass peak of SiF3+ produced by the etching of the Si substrate.

  19. Rapid quantification of the metabolite of valacyclovir hydrochloride in human plasma by liquid chromatography-tandem mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Objective To establish a rapid,sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of acyclovir (the metabolite of valacyclovir hydrochloride) in human plasma. Methods After addition of ganciclovir as internal standard (IS),plasma samples were prepared by one-step protein precipitation using acetonitrile as precipitant,followed by an isocratic elution with 0.1% formic acid solution-methanol (95∶5,v/v) on an Agilent ZORBAX SB-C18 (150mm×2.1mm i.d.,3....

  20. A new method of measuring the spatial distribution of depletion fraction of silane plasma by mass spectrometer

    Institute of Scientific and Technical Information of China (English)

    Wang Zhao-Kui; Lin Kui-Xun; Lin Xuan-Ying; Qiu Gui-Ming; Zhu Zu-Song

    2005-01-01

    A newly established movable sampling apparatus of mass spectrometer is used to measure the spatial distribution of depletion fraction of silane plasma. A straight-line fit method of deducing the depletion fraction of silane is proposed.Theoretical analysis and test results demonstrate that the proposed new method is universal and more accurate than the existing one. There exist a largest peak near the middle of two electrodes and two peaks near the electrodes in the spatial distribution of silane depletion fraction, which are related to the distribution of electric field and the silane plasma sheaths.

  1. Multifluid MHD simulation of Saturn's magnetosphere: Dynamics of mass- and momentum-loading, and seasonal variation of the plasma sheet

    Science.gov (United States)

    Rajendar, A.; Paty, C. S.; Arridge, C. S.; Jackman, C. M.; Smith, H. T.

    2013-12-01

    Saturn's magnetosphere is driven externally, by the solar wind, and internally, by the planet's strong magnetic field, rapid rotation rate, and the addition of new plasma created from Saturn's neutral cloud. Externally, the alignment of the rotational and magnetic dipole axes, combined with Saturn's substantial inclination to its plane of orbit result in substantial curvature of the plasma sheet during solstice. Internally, new water group ions are produced in the inner regions of the magnetosphere from photoionization and electron-impact ionization of the water vapor and OH cloud sourced from Enceladus and other icy bodies in Saturn's planetary system. In addition to this, charge-exchange collisions between the relatively fast-moving water group ions and the slower neutrals results in a net loss of momentum from the plasma. In order to study these phenomena, we have made significant modifications to the Saturn multifluid model. This model has been previously used to investigate the external triggering of plasmoids and the interchange process using a fixed internal source rate. In order to improve the fidelity of the model, we have incorporated a physical source of mass- and momentum-loading by including an empirical representation of Saturn's neutral cloud and modifying the multifluid MHD equations to include mass- and momentum-loading terms. Collision cross-sections between ions, electrons, and neutrals are calculated as functions of closure velocity and energy at each grid point and time step, enabling us to simulate the spatially and temporally varying plasma-neutral interactions. In addition to this, by altering the angle of incidence of the solar wind relative to Saturn's rotational axis and applying a realistic latitudinally- and seasonally-varying ionospheric conductivity, we are also able to study seasonal effects on Saturn's magnetosphere. We use the updated multifluid simulation to investigate the dynamics of Saturn's magnetosphere, focusing specifically

  2. Effect of fat free mass on serum and plasma BDNF concentrations during exercise and recovery in healthy young men.

    Science.gov (United States)

    Gilder, M; Ramsbottom, R; Currie, J; Sheridan, B; Nevill, A M

    2014-02-07

    Exercise results in release of brain derived neurotrophic factor into the circulation; however, little is known about the changes in serum and plasma brain derived neurotrophic factor concentrations and factors influencing brain derived neurotrophic factor during exercise and recovery. Serum (n=23) and plasma (n=10) brain derived neurotrophic factor concentrations were measured in healthy young men at rest, during steady-rate and after exercise to determine the maximum aerobic power. A two-way analysis of variance was used to investigate brain derived neurotrophic factor levels in blood during exercise and recovery, with one between-subject factor (a median split on: age, height, body mass, fat free mass, body mass index and aerobic fitness), and one within-subject factor (time). Serum brain derived neurotrophic factor concentrations increased in response to exercise and declined rapidly in recovery. Plasma brain derived neurotrophic factor had a greater proportional increase relative to exhaustive exercise compared with serum brain derived neurotrophic factor and was slower to return to near baseline values. There was a significant group-by-time interaction indicating a greater release and faster recovery for serum brain derived neurotrophic factor in high- compared with low-fat free mass individuals.

  3. Validation of a simple gas chromatographic-mass spectrometric method for the determination of gamma-butyrolactone in human plasma.

    Science.gov (United States)

    Fukui, Yousuke; Matsusima, Eiji; Muramoto, Kouichi; Nagai, Nobutaka; Ohama, Koso; Yamashita, Kazumasa

    2003-02-25

    A gas chromatographic-mass spectrometric (GC-MS) method is described for the determination of human plasma levels of gamma-butyrolactone (GBL) is described. The method is sensitive and simple. The plasma sample spiked with the internal standard was extracted by dichloromethane (CH(2)Cl(2)) in acidic conditions, and the concentrated organic layer was injected into GC-MS. Because of endogenous GBL in human plasma, the method used a standard calibration curve. The calibration curve was linear from 10 to 1000 ng/ml. The method has been validated for accuracy and precision with the relative error and C.V. for intra- and inter-day within 10%. GBL-spiked plasma samples stored at -80 degrees C were stable for a 3-month period. The stability of plasma samples after three cycles of freezing and thawing and of prepared samples on an autosampler for 48 h were demonstrated. Plasma concentrations of GBL before and after administration of UFT were 24.3+/-14.2 and 84.9+/-22.4 ng/ml, respectively.

  4. Determination of uranium from nuclear fuel in environmental samples using inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, S.F. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen]|[Radiation Physics and Chemistry Problems Inst., Minsk (Belarus); Becker, J.S. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen

    2000-11-01

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The {sup 236}U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A {sup 238}U{sup +} ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min{sup -1}. The formation rate of uranium hydride ions UH{sup +}/U{sup +} of 2 x 10{sup -6} was obtained by using USN with a membrane desolvator. The limit of {sup 236}U/{sup 238}U ratio determination in 10 {mu}g 1{sup -1} uranium solution was 3 x 10{sup -7} corresponding to the detection limit for {sup 236}U of 3 pg 1{sup -1}. The precision of uranium isotopic ratio measurements in 10 {mu}g 1{sup -1} laboratory uranium isotopic standard solution was 0.13% ({sup 235}U/{sup 238}U) and 0.33% ({sup 236}U/{sup 238}U) using a Meinhard nebulizer and 0.45% ({sup 235}U/{sup 238}U) and 0.88% ({sup 236}U/{sup 238}U) using a USN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the {sup 236}U/{sup 238}U ratio ranged from 10{sup -5} to 10{sup -3}. (orig.)

  5. Influence of instrumental parameters on the kinetic energy of ions and plasma temperature for a hexapole collision/reaction-cell-based inductively coupled plasma quadrupole mass spectrometer.

    Science.gov (United States)

    Favre, Georges; Brennetot, René; Chartier, Frédéric; Tortajada, Jeanine

    2009-02-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in inorganic analytical chemistry for element and/or isotope ratio measurements. The presence of interferences, which is one of the main limitations of this method, has been addressed in recent years with the introduction of collision/reaction cell devices on ICP-MS apparatus. The study of ion-molecule reactions in the gas phase then became of great importance for the development of new analytical strategies. Knowing the kinetic energy and the electronic states of the ions prior to their entrance into the cell, i.e., just before they react, thereby constitutes crucial information for the interpretation of the observed reactivities. Such studies on an ICP-MS commonly used for routine analyses require the determination of the influence of different instrumental parameters on the energy of the ions and on the plasma temperature from where ions are sampled. The kinetic energy of ions prior to their entrance into the cell has been connected to the voltage applied to the hexapole according to a linear relationship determined from measurements of ion energy losses due to collisions with neutral gas molecules. The effects of the plasma forward power, sampling depth, and the addition of a torch shield to the ICP source were then examined. A decrease of the plasma potential due to the torch shielding, already mentioned in the literature, has been quantified in this study at about 3 V.

  6. Developments in and applications of capillary electrophoresis inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Taylor, K.A

    1999-08-01

    This project has set out to design and optimise a robust and efficient interface for capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) and to investigate the application of the technique in elemental speciation studies. An interface was constructed using a commercial microconcentric nebuliser (MCN) and a cyclonic spray chamber. The cyclonic spray chamber was designed specifically to provide rapid sample response and washout and to minimise sample dispersion. Isoforms of the heavy metal binding protein, metallothionein, were separated and the bound metals detected to characterise the interface. Suction from the self-aspirating nebuliser was identified as the principal factor controlling electrophoretic resolution. To maintain resolution, two methods for counterbalancing the nebuliser suction were investigated. In the first method an optimised make-up flow was employed, and in the second a negative pressure was applied to the buffer vial during the separation. The negative pressure method was preferred because it did not significantly compromise sensitivity. The MCN was found to be prone to regular blocking which compromised the analytical precision of the system. A second interface was constructed using a glass MicroMist nebuliser. The MicroMist nebuliser was found to be less prone to blocking than the MCN and significantly improved the precision of the system to less than 4.3% RSD. The MicroMist nebuliser did, however, provide a lower sensitivity. The advantage of employing an electroosmotic flow marker to correct for migration time drifts was demonstrated. A CE-ICP-MS method was developed for the speciation of selenium in selenium enriched yeasts and nutritional supplements. Selenoamino acids and inorganic selenium species were separated, as anions, under strong electroosmotic flow conditions. Methods to enhance the selenium sensitivity were investigated. A proteolytic enzyme extraction method was employed and the effect of the

  7. Identification of organically associated trace elements in wood and coal by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Richaud, R; Lazaro, M J; Lachas, H; Miller, B B; Herod, A A; Dugwell, D R; Kandiyoti, R

    2000-01-01

    1-Methyl-2-pyrrolidinone (NMP) was used to extract samples of wood (forest residue) and coal; the extracts were analysed by inductively coupled plasma mass spectrometry (ICP-MS) using two different sample preparation methods, in order to identify trace elements associated with the organic part of the samples. A sample of fly ash was similarly extracted and analysed in order to assess the behaviour of the mineral matter contained within the wood and coal samples. 32% of the biomass was extracted at the higher temperature and 12% at room temperature while only 12% of the coal was extracted at the higher temperature and 3% at room temperature. Less than 2% of the ash dissolved at the higher temperature. Size exclusion chromatograms of the extracts indicated the presence of significant amounts of large molecular mass materials (>1000 mu) in the biomass and coal extracts but not in the ash extract. Trace element analyses were carried out using ICP-MS on the acid digests prepared by 'wet ashing' and microwave extraction. Sixteen elements (As, Ba, Be, Cd, Co, Cr, Cu, Ga, Mn, Mo, Ni, Pb, Sb, Se, V and Zn) were quantified, in the samples before extraction, in the extracts and in the residues. Concentrations of trace elements in the original biomass sample were lower than in the coal sample while the concentrations in the ash sample were the highest. The major trace elements in the NMP extracts were Ba, Cu, Mn and Zn from the forest residue; Ba, Cu, Mn, Pb and Zn from the coal; Cu and Zn from the ash. These elements are believed to be associated with the organic extracts from the forest residue and coal, and also from the ash. Be and Sb were not quantified in the extracts because they were present at too low concentrations; up to 40% of Mn was extracted from the biomass sample at 202 degrees C, while Se was totally extracted from the ash sample. For the forest residue, approximately 7% (at room temperature) and 45% (at 202 degrees C) of the total trace elements studied were

  8. Quantitative analysis of [Dmt(1)]DALDA in ovine plasma by capillary liquid chromatography-nanospray ion-trap mass spectrometry.

    Science.gov (United States)

    Wan, Haibao; Umstot, Edward S; Szeto, Hazel H; Schiller, Peter W; Desiderio, Dominic M

    2004-04-15

    The synthetic opioid peptide analog Dmt-D-Arg-Phe-Lys-NH(2) ([Dmt(1)]DALDA; [Dmt= 2',6'-dimethyltyrosine) is a highly potent and selective mu opioid-receptor agonist. A very sensitive and robust capillary liquid chromatography/nanospray ion-trap (IT) mass spectrometry method has been developed to quantify [Dmt(1)]DALDA in ovine plasma, using deuterated [Dmt(1)]DALDA as the internal standard. The standard MS/MS spectra of d(0)- and d(5)-[Dmt(1)]DALDA were obtained, and the collision energy was experimentally optimized to 25%. The product ion [ M + 2H-NH(3)](2+) (m/z 312.2) was used to identify and to quantify the synthetic opioid peptide analog in ovine plasma samples. The MS/MS detection sensitivity for [Dmt(1)]DALDA was 625 amol. A calibration curve was constructed, and quantitative analysis was performed on a series of ovine plasma samples.

  9. Photochemical vapor generation of lead for inductively coupled plasma mass spectrometric detection

    Science.gov (United States)

    Duan, Hualing; Zhang, Ningning; Gong, Zhenbin; Li, Weifeng; Hang, Wei

    2016-06-01

    Photochemical vapor generation (PCVG) of lead was successfully achieved with a simplified and convenient system, in which only low molecular weight organic acid and a high-efficiency photochemical reactor were needed. The reactor was used to generate lead volatile species when a solution of lead containing a small amount of low molecular weight organic acid was pumped through. Several factors, including the concentration of acetic acid, the concentration of hydrochloride acid, and the irradiation time of UV light were optimized. Under the optimal conditions, including the addition of 0.90% (v/v) acetic acid and 0.03% (v/v) hydrochloride acid, and irradiation time of 28 s, intense and repeatable signal of lead volatile species was successfully obtained and identified with inductively coupled plasma mass spectrometry (ICPMS). In addition, the effects from inorganic anions and transition metal ions, including Cl-, NO3-, SO42 -, Cu2 +, Fe3 +, Co2 + and Ni2 +, were investigated, which suggests that their suppression to the PCVG of lead was in the order of Cl- anions and Ni2 +, Co2 + < Fe3 + < Cu2 + for transition metal ions. Under optimized conditions, relative standard derivation (RSD) of 4.4% was achieved from replicate measurements (n = 5) of a standard solution of 0.1 μg L- 1 lead. And, the limit of quantitation (LOQ, 10σ) of 0.012 μg L- 1 lead was obtained using this method and the method blank could be easily controlled down to 0.023 μg L- 1. To validate applicability of this method, it was also employed for the determination of lead in tap water, rain water and lake water.

  10. Documenting utility of paddlefish otoliths for quantification of metals using inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Long, James M.; Schaffler, James J.

    2013-01-01

    RATIONALE The otoliths of the inner ear of fishes record the environment of their surrounding water throughout their life. For paddlefish (Polyodon spathula), otoliths have not been routinely used by scientists since their detriments were outlined in the early 1940s. We sought to determine if paddlefish otoliths were useful for resolving elemental information contained within. METHODS Adult paddlefish were collected from two wild, self-sustaining populations in Oklahoma reservoirs in the Arkansas River basin. Juveniles were obtained from a hatchery in the Red River basin of Oklahoma. Otoliths were removed and laser ablation, inductively coupled plasma mass spectrometry (ICP-MS) was used to quantify eight elements (Li, Mg, Mn, Rb, Sr, Y, Ba, and Pb) along the core and edge portions, which were analyzed for differences between otolith regions and among paddlefish sources. RESULTS Differences were found among samples for six of the eight elements examined. Otoliths from Red River basin paddlefish born in a hatchery had significantly lower amounts of Mg and Mn, but higher levels of Rb than otoliths from wild paddlefish in the Arkansas River basin. Concentrations of Y, Sr, and Ba were reduced on the edges of adult paddlefish from both reservoirs compared with the cores. CONCLUSIONS This research shows the utility of using an ICP-MS analysis of paddlefish otoliths. Future research that seeks to determine sources of paddlefish production, such as which reservoir tributaries are most important for reproduction or what proportion of the population is composed of wild versus hatchery-produced individuals, appears promising. Published in 2013. This article is a U.S. Government work and is in the public domain in the USA.

  11. Detecting nanoparticulate silver using single-particle inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Mitrano, Denise M; Lesher, Emily K; Bednar, Anthony; Monserud, Jon; Higgins, Christopher P; Ranville, James F

    2012-01-01

    The environmental prevalence of engineered nanomaterials, particularly nanoparticulate silver (AgNP), is expected to increase substantially. The ubiquitous use of commercial products containing AgNP may result in their release to the environment, and the potential for ecological effects is unknown. Detecting engineered nanomaterials is one of the greatest challenges in quantifying their risks. Thus, it is imperative to develop techniques capable of measuring and characterizing exposures, while dealing with the innate difficulties of nanomaterial detection in environmental samples, such as low-engineered nanomaterial concentrations, aggregation, and complex matrices. Here the authors demonstrate the use of inductively coupled plasma-mass spectrometry, operated in a single-particle counting mode (SP-ICP-MS), to detect and quantify AgNP. In the present study, two AgNP products were measured by SP-ICP-MS, including one of precisely manufactured size and shape, as well as a commercial AgNP-containing health food product. Serial dilutions, filtration, and acidification were applied to confirm that the method detected particles. Differentiation of dissolved and particulate silver (Ag) is a feature of the technique. Analysis of two wastewater samples demonstrated the applicability of SP-ICP-MS at nanograms per liter Ag concentrations. In this pilot study, AgNP was found at 100 to 200 ng/L in the presence of 50 to 500 ng/L dissolved Ag. The method provides the analytical capability to monitor Ag and other metal and metal oxide nanoparticles in fate, transport, stability, and toxicity studies using a commonly available laboratory instrument. Rapid throughput and element specificity are additional benefits of SP-ICP-MS as a measurement tool for metal and metal oxide engineered nanoparticles. Copyright © 2011 SETAC.

  12. Determination of minor elements in steelmaking flue dusts using laser ablation inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Coedo, A G; Padilla, I; Dorado, M T

    2005-07-15

    Element determination in solid waste products from the steel industry usually involves the time-consuming step of preparing a solution of the solid. Laser ablation (LA) inductively coupled plasma mass spectrometry (ICP-MS) has been applied to the analysis of Cr, Ni, Cu, As, Cd and Sn, elements of importance from the point of view of their impact on the environment, in electric arc furnace flue dust (EAFD). A simple method of sample preparation as pressed pellets using a mixture of cellulose and paraffin as binder material was applied. Calibration standards were prepared spiking multielement solution standards to a 1:1 ZnO+Fe(2)O(3) synthetic matrix. The wet powder was dried and mechanically homogenised. Quantitative analysis were based on external calibration using a set of matrix matched calibration standards with Rh as a internal standard. Results obtained using only one-point for calibration without matrix matched, needing less time for standardization and data processing, are also presented. Data are calculated for flue dust reference materials: CRM 876-1 (EAFD), AG-6203 (EAFD), AG-6201 (cupola dust) and AG-SX3705 (coke ashes), and for two representative electrical arc furnace flue dusts samples from Spanish steelmaking companies: MS-1 and MS-2. For the reference materials, an acceptable agreement with certificate values was achieved, and the results for the MS samples matched with those obtained from conventional nebulization solutions (CN). The analytical precision was found to be better than 7% R.S.D. both within a single pellet and between several pellets of the same sample for all the elements.

  13. Analysis of liquid samples using dried-droplet laser ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Do, Trong-Mui; Hsieh, Hui-Fang; Chang, Wei-Ciang [Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu, 30013 Taiwan (China); Chang, E.-E. [Department of Biochemistry, Taipei Medical University, Taipei City, 11031 Taiwan (China); Wang, Chu-Fang, E-mail: cfwang@mx.nthu.edu.tw [Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu, 30013 Taiwan (China); Institute of Nuclear Engineering and Science, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

    2011-08-15

    In this study we developed a dried-droplet method for laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method provides accurate and precise results when building calibration curves and determining elements of interest in real liquid samples. After placing just 1 {mu}L of a liquid standard solution or a real sample onto the filter surface and then converting the solution into a very small, thin dry spot, the sample could be applied as an analytical subject for LA. To demonstrate the feasibility of this proposed method, we used LA-ICP-MS and conventional ICP-MS to determine the levels of 13 elements (Li, V, Mn, Co, Ni, Cu, Zn, As, Mo, Cd, Sb, Tl, and Pb) in five water samples. The correlation coefficients obtained from the various calibration curves ranged from 0.9920 ({sup 205}Tl) to 0.9998 ({sup 51}V), sufficient to allow the determination of a wide range of elements in the samples. We also investigated the effects of Methylene Blue (MB) and the NaCl concentration on the elemental analyses. MB could be used as an indicator during the ablation process; its presence in the samples only negligibly influenced the intensities of the signals of most of the tested elements. Notably, high NaCl contents led to signal suppression for some of the elements. In comparison with the established sample introduction by nebulization, our developed technique abrogates the need for time-consuming sample preparation and reduces the possibility of sample contamination.

  14. ISEE-3 observations of a viscously-driven plasma sheet: magnetosheath mass and/or momentum transfer?

    Science.gov (United States)

    Mist, R. T.; Owen, C. J.

    2002-05-01

    A statistical analysis of data from the ISEE-3 distant tail campaign is presented. We investigate the mechanism driving slow, tailward flows observed in the plasma sheet. The possibility that these slow flows are driven by mass and/or momentum transfer across the distant tail magnetopause is explored. We establish that 40% of these flows could be driven by the transfer of approximately 4% of the magnetosheath momentum flux into the magnetotail. Current understanding of the Kelvin-Helmholtz instability suggests that this figure is consistent with the amount of momentum flux transfer produced by this mechanism. We also consider the possibility that these flows are solely driven by transferring magnetosheath plasma across the magnetopause. We find that there is sufficient mass observed on these field lines for this to be the sole driving mechanism for only 27% of the observed slow flows.

  15. Measurement of pyrethroid, organophosphorus, and carbamate insecticides in human plasma using isotope dilution gas chromatography-high resolution mass spectrometry.

    Science.gov (United States)

    Pérez, José J; Williams, Megan K; Weerasekera, Gayanga; Smith, Kimberly; Whyatt, Robin M; Needham, Larry L; Barr, Dana Boyd

    2010-10-01

    We have developed a gas chromatography-high resolution mass spectrometry method for measuring pyrethroid, organophosphorus, carbamate and fipronil pesticides and the synergist piperonyl butoxide in human plasma. Plasma samples were extracted using solid phase extraction and were then concentrated for injection and analysis using isotope dilution gas chromatography-high resolution mass spectrometry. The limits of detection ranged from 10 to 158 pg/mL with relative recoveries at concentrations near the LODs (e.g., 25 or 250 pg/mL) ranging from 87% to 156% (9 of the 16 compounds were within ±15% of 100%). The extraction recoveries ranged from 20% to 98% and the overall method relative standard deviations were typically less than 20% with some exceptions. Analytical characteristics were determined at 25, 250, and 1000 pg/mL.

  16. Determination of Rare Earth Elements in Green River Shale By Inductively Coupled Plasma Mass Spectrometry Using a Desolvating Nebulizer System

    Science.gov (United States)

    Smith, F.; Clarke, D.; Moody, S.

    2014-12-01

    In this work, inductively coupled plasma mass spectrometry (ICP-MS) is applied to a geological sample for the determination of rare earth elements (REEs) using a specialized nebulizer system. The low flow desolvating nebulizer has been shown to decrease metal oxide formation which leads to a reduction in mass spectral interferences. Traditional nebulizers and spray chambers may be suitable for similar sample types, but reduction of water vapor loading to the plasma can improve REE detection limits for quadrupole-based ICP-MS. The Green River formation holds the largest oil shale deposits in the world and understanding the elemental composition of these samples is important in its study. A certified reference material, USGS Green River Shale (SGR-1), was microwave digested prior to analysis, and recoveries of REEs compared to historical values are discussed.

  17. Fractionation analysis of manganese in Turkish hazelnuts (Corylus avellana L.) by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Erdemir, Umran Seven; Gucer, Seref

    2014-11-05

    In this study, an analytical fractionation scheme based on water, diethyl ether, n-hexane, and methanol extractions has been developed to identify manganese-bound fractions. Additionally, in vitro simulated gastric and intestinal digestion, n-octanol extraction, and activated carbon adsorption were used to interpret the manganese-bound structures in hazelnuts in terms of bioaccessibility. The total content of manganese in the samples was determined by inductively coupled plasma-mass spectrometry after microwave-assisted digestion, and additional validation was performed using atomic absorption spectroscopy. Water fractions were further evaluated by high-performance liquid chromatography hyphenated to inductively coupled plasma-mass spectrometry for the identification of water-soluble manganese fractions in hazelnut samples. The limits of detection and quantification were 3.6 and 12.0 μg L(-1), respectively, based on peak height.

  18. Direct tandem mass spectrometric analysis of amino acids in plasma using fluorous derivatization and monolithic solid-phase purification.

    Science.gov (United States)

    Tamashima, Erina; Hayama, Tadashi; Yoshida, Hideyuki; Imakyure, Osamu; Yamaguchi, Masatoshi; Nohta, Hitoshi

    2015-11-10

    In this study, we developed a novel direct tandem mass spectrometric method for rapid and accurate analysis of amino acids utilizing a fluorous derivatization and purification technique. Amino acids were perfluoroalkylated with 2H,2H,3H,3H-perfluoroundecan-1-al in the presence of 2-picoline borane via reductive amination. The derivatives were purified by perfluoroalkyl-modified silica-based monolithic solid-phase extraction (monolithic F-SPE), and directly analyzed by tandem mass spectrometry using electrospray ionization without liquid chromatographic separation. The perfluoroalkyl derivatives could be sufficiently distinguished from non-fluorous compounds, i.e. the biological matrix, due to their fluorous interaction. Thus, rapid and accurate determination of amino acids was accomplished. The method was validated with human plasma samples and applied to the analysis of amino acids in the plasma of mice with maple syrup urine disease or phenylketonuria.

  19. Femtosecond laser ablation: Experimental study of the repetition rate influence on inductively coupled plasma mass spectrometry performance

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez, Jhanis J. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Fernandez, Alberto [Centro de Fisicoquimica. Escuela de Quimica, Universidad Central de Venezuela, Caracas 1020-A (Venezuela); Oropeza, Dayana; Mao Xianglei [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Russo, Richard E. [Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States)], E-mail: RERusso@lbl.gov

    2008-02-15

    This paper demonstrates the feasibility of performing bulk chemical analysis based on laser ablation for good lateral resolution with only nominal mass ablated per pulse. The influence of repetition rate (1-1000 Hz) and scan speed (1-200 {mu}m/s) using a low energy (30 {mu}J) and a small spot size ({approx} 10 {mu}m) UV-femtosecond laser beam was evaluated for chemical analysis of silica glass samples, based on laser ablation sampling and inductively coupled plasma mass spectrometry (ICP-MS). Accuracy to approximately 14% and precision of 6% relative standard deviation (RSD) were measured.

  20. Effect of ion mass on pair production in the interaction of an ultraintense laser with overdense plasmas

    CERN Document Server

    Wan, F; Jia, M R; Wang, H Y; Xie, B S

    2016-01-01

    The effect of ion mass on pair production in the interaction of an ultraintense laser with overdense plasmas has been explored by particle-in-cell (PIC) simulation. It is found that the heavier ion mass excites the higher and broader electrostatic field, which is responsible for the enhancement of backward photon number. The pair yields are also reinforced due to the increase of head-on collision of backwards photon with incoming laser. By examining the density evolution and angle distribution of each particle species the origin of pair yields enhancement has been clarified further.

  1. ISEE-3 observations of a viscously-driven plasma sheet: magnetosheath mass and/or momentum transfer?

    OpenAIRE

    Mist, R. T.; Owen, C.J.

    2002-01-01

    A statistical analysis of data from the ISEE-3 distant tail campaign is presented. We investigate the mechanism driving slow, tailward flows observed in the plasma sheet. The possibility that these slow flows are driven by mass and/or momentum transfer across the distant tail magnetopause is explored. We establish that 40% of these flows could be driven by the transfer of approximately 4% of the magnetosheath momentum flux into the magnetotail. Current understanding of the Kelvin-Helmholtz in...

  2. ISEE-3 observations of a viscously-driven plasma sheet: magnetosheath mass and/or momentum transfer?

    OpenAIRE

    Mist, R. T.; Owen, C.J.

    2002-01-01

    A statistical analysis of data from the ISEE-3 distant tail campaign is presented. We investigate the mechanism driving slow, tailward flows observed in the plasma sheet. The possibility that these slow flows are driven by mass and/or momentum transfer across the distant tail magnetopause is explored. We establish that 40% of these flows could be driven by the transfer of approximately 4% of the magnetosheath momentum flux into the magnetotail. Current understanding of the Kelvin-Helmh...

  3. The equilibrium of the dense electron-nuclear plasma in the gravitational field. The magnetic fields and masses of stars

    CERN Document Server

    Vasilev, B V

    2003-01-01

    The equilibrium of a hot dense plasma in a gravitational field is considered. From the standard equilibrium equations, the energy minimum at density about $10^{25}$ particles per $cm^3$ and temperature about $10^7 K$ was found. This effect plays an important role for astrophysics. It enables to explain the mechanism of the star magnetic field generation and to make a prediction for the spectrum of a star mass with a wholly satisfactory agreement for the observation data.

  4. Determination of the species generated in atmospheric-pressure laser-induced plasmas by mass spectrometry techniques

    CERN Document Server

    Valle, F; Apiñaniz, J I; Carpentier, A V; Albaneda, M Sánchez; Roso, L; Raposo, C; Padilla, C; Conde, A Peralta

    2015-01-01

    We present temporal information obtained by mass spectrometry techniques about the evolution of plasmas generated by laser filamentation in air. The experimental setup used in this work allowed us to study not only the dynamics of the filament core but also of the energy reservoir that surrounds it. Furthermore, valuable insights about the chemistry of such systems like the photofragmentation and/or formation of molecules were obtained. The interpretation of the experimental results are supported by PIC (particle in cell) simulations.

  5. Application of inductively coupled plasma quadrupole mass spectrometry for the determination of monazite ages by lead isotope ratios

    OpenAIRE

    Godoy,José Marcus; Godoy,Maria Luiza D. P; Aronne,Cláudia C.

    2007-01-01

    In order to evaluate the applicability of inductively coupled plasma quadrupole mass spectrometry to the determination of Pb/Pb, U/Pb and Th/Pb ages of monazite, studies were carried out initially applying lead atom ratio reference standards (NIST SRM 981 and 982). Further, the optimized methodology was applied to monazite sands from three different sites, Sugar Loaf Hill (Rio de Janeiro city), Buena (Rio de Janeiro state) and Black Sands Beach (Guarapari, Espirito Santo state); the obtained ...

  6. Quantitation of drugs via molecularly imprinted polymer solid phase extraction and electrospray ionization mass spectrometry: benzodiazepines in human plasma

    OpenAIRE

    2011-01-01

    The association of solid phase extraction with molecularly imprinted polymers (MIP) and electrospray ionization mass spectrometry (ESI-MS) is applied to the direct extraction and quantitation of benzodiazepines in human plasma. The target analytes are sequestered by MIP and directly analyzed by ESI-MS. Due to the MIP highly selective extraction, ionic suppression during ESI is minimized; hence no separation is necessary prior to ESI-MS, which greatly increases analytical speed. Benzodiazepine...

  7. Determining transport efficiency for the purpose of counting and sizing nanoparticles via single particle inductively coupled plasma-mass spectrometry

    OpenAIRE

    Pace, Heather E.; Rogers, Nicola J.; Jarolimek, Chad; Coleman, Victoria A.; Higgins, Christopher P.; Ranville, James F.

    2011-01-01

    Currently there are few ideal methods for the characterization of nanoparticles in complex, environmental samples, leading to significant gaps in toxicity and exposure assessments of nanomaterials. Single particle-inductively coupled plasma-mass spectrometry (spICP-MS) is an emerging technique that can both size and count metal-containing nanoparticles. A major benefit of the spICP-MS method is its ability to characterize nanoparticles at concentrations relevant to the environment. This paper...

  8. Determination of Ephedrine Alkaloids in Human Urine and Plasma by Liquid Chromatography/Tandem Mass Spectrometry: Collaborative Study

    Science.gov (United States)

    Trujillo, William A.; Sorenson, Wendy R.

    2008-01-01

    A collaborative study was conducted to evaluate the accuracy and precision of a method for ephedrine-type alkaloids (i.e., norephedrine, norpseudoephedrine, ephedrine, pseudoephedrine, methylephedrine, and methylpseudoephedrine) in human urine and plasma. The amount of ephedrine-type alkaloids present was determined using liquid chromatography (LC) with tandem mass selective detection. The test samples were diluted to reflect a concentration of 5.00–100 ng/mL for each alkaloid. An internal standard was added and the alkaloids were separated using a 5 μm phenyl LC column with an ammonium acetate, glacial acetic acid, acetonitrile, and water mobile phase. Eight blind duplicates of human urine and eight blind duplicates of human plasma were analyzed by 10 collaborators. In addition to negative controls, test portions of urine and plasma were fortified at 3 different levels with each of the 6 ephedrine-type alkaloids at approximately 1, 2, and 5 μg/mL for urine and 100, 200, and 500 ng/mL for plasma. On the basis of the accuracy and precision results for this collaborative study, it is recommended that this method be adopted Official First Action for the determination of 6 different ephedrine-type alkaloids in human urine and plasma. PMID:14509420

  9. Effect of piperine on pharmacokinetics of sodium valproate in plasma samples of rats using gas chromatography-mass spectrometry method

    Directory of Open Access Journals (Sweden)

    Bushra Parveen

    2015-01-01

    Full Text Available Piperine (PIP is used as anticonvulsant in traditional Chinese medicine. Co-administration of low-dose sodium valproate with PIP has been regarded to have potential anticonvulsant activity. Aim: This study was intended to investigate the effect of PIP on the pharmacokinetics of sodium valproate (SVP in the plasma samples of rats using gas chromatography-mass spectrometry (GC-MS method. Materials and Methods: The plasma samples obtained after oral administration of SVP, 150 mg/kg and SVP, 150 mg/kg + PIP, and 5 mg/kg to male Wistar rats were used to quantify the concentrations in plasma using GC-MS method. Results: A simple and accurate method developed in-house was applied for the analysis of plasma samples of Wistar rats after oral administration of SVP and PIP + sodium valproate, respectively. The pharmacokinetic parameters reported 14.8-fold increase in plasma concentration (maximum observed concentration in the concentration-time profile, 4.6-fold increase in area under the curve and slightly prolonged time to reach that concentration (1 h of SVP in presence of PIP. Conclusion: The study reaffirms the bioenhancing effect of PIP suggesting possibility of dose reduction of SVP while co-adminstering with PIP.

  10. Endogenous Plasma Peptide Detection and Identification in the Rat by a Combination of Fractionation Methods and Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Fabrice Bertile

    2007-01-01

    Full Text Available Mass spectrometry-based analyses are essential tools in the field of biomarker research. However, detection and characterization of plasma low abundance and/or low molecular weight peptides is challenged by the presence of highly abundant proteins, salts and lipids. Numerous strategies have already been tested to reduce the complexity of plasma samples. The aim of this study was to enrich the low molecular weight fraction of rat plasma. To this end, we developed and compared simple protocols based on membrane filtration, solid phase extraction, and a combination of both. As assessed by UV absorbance, an albumin depletion 99% was obtained. The multistep fractionation strategy (including reverse phase HPLC allowed detection, in a reproducible manner (CV [1] 30%–35%, of more than 450 peaks below 3000 Da by MALDI-TOF/MS. A MALDI-TOF/MS-determined LOD as low as 1 fmol/μL was obtained, thus allowing nanoLC-Chip/ MS/MS identification of spiked peptides representing ∼10–6% of total proteins, by weight. Signal peptide recovery ranged between 5%–100% according to the spiked peptide considered. Tens of peptide sequence tags from endogenous plasma peptides were also obtained and high confidence identifications of low abundance fibrinopeptide A and B are reported here to show the efficiency of the protocol. It is concluded that the fractionation protocol presented would be of particular interest for future differential (high throughput analyses of the plasma low molecular weight fraction.

  11. Large molecular mass materials in coal-derived liquids by {sup 252}Cf-plasma and matrix-assisted laser desorption mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Domin, M.; Li, S.; Lazaro, M.-J.; Herod, A.A.; Larsen, J.W.; Kandiyoti, R. [School of Pharmacy, London (United Kingdom). Dept. of Parmaceutical and Biological Chemistry

    1998-05-01

    The paper compares responses of {sup 252}Cf-plasma desorption MS (PD-MS) and matrix-assisted laser desorption (MALDI) MS to identical samples. The two pairs of samples selected for the comparison were known from previous work to differ significantly in their high mass contents. MALDI-MS showed large differences in MM distributions within both pairs of samples. The PD-MS data showed a degree of similarity between one pair of samples (pyridine soluble/insoluble fractions of a coal tar pitch); for the second pair (a coal extract and its hydrocracked product), trends from the two MS techniques agreed closely. The MM range observed by PD-MS was somewhat narrower, extending to between 3000 and 5000 u. Significant differences within pairs of samples were observed by SEC and by UV-fluorescence spectroscopy, providing somewhat closer agreement with the MALDI spectra. The two MS instruments differ in two important respects: the ionization system (i.e., plasma vs laser desorption) and the maximum available ion extraction voltage: 30 kV for the MALDI-MS instrument and 15 kV for the PD-MS. The comparison of plasma vs laser desorption mass spectroscopy could not therefore take place at high ion extraction voltages. Work at up to 30 kV in the MALDI instrument indicated better sensitivity to high-mass materials at higher ion extraction voltages. The qualitative similarity of results from the two MS techniques is nevertheless apparent; the range of MMs observed in PD-MS as well as in MALDI-MS were, furthermore, far larger than those reported by any MS technique, to date. 38 refs., 6 figs., 1 tab.

  12. Characterization of the human plasma phosphoproteome using linear ion trap mass spectrometry and multiple search engines.

    Science.gov (United States)

    Carrascal, Montserrat; Gay, Marina; Ovelleiro, David; Casas, Vanessa; Gelpí, Emilio; Abian, Joaquin

    2010-02-05

    Major plasma protein families play different roles in blood physiology and hemostasis and in immunodefense. Other proteins in plasma can be involved in signaling as chemical messengers or constitute biological markers of the status of distant tissues. In this respect, the plasma phosphoproteome holds potentially relevant information on the mechanisms modulating these processes through the regulation of protein activity. In this work we describe for the first time a collection of phosphopeptides identified in human plasma using immunoaffinity separation of the seven major serum protein families from other plasma proteins, SCX fractionation, and TiO(2) purification prior to LC-MS/MS analysis. One-hundred and twenty-seven phosphosites in 138 phosphopeptides mapping 70 phosphoproteins were identified with FDR < 1%. A high-confidence collection of phosphosites was obtained using a combined search with the OMSSA, SEQUEST, and Phenyx search engines.

  13. Tellurium isotopic composition of the early solar system—A search for effects resulting from stellar nucleosynthesis, 126Sn decay, and mass-independent fractionation

    Science.gov (United States)

    Fehr, Manuela A.; Rehkämper, Mark; Halliday, Alex N.; Wiechert, Uwe; Hattendorf, Bodo; Günther, Detlef; Ono, Shuhei; Eigenbrode, Jennifer L.; Rumble, Douglas

    2005-11-01

    New precise Te isotope data acquired by multiple collector inductively coupled plasma mass spectrometry (MC-ICPMS) are presented for selected extraterrestrial and terrestrial materials. Bulk samples of carbonaceous, ordinary and enstatite chondrites as well as the metal and sulfide phases of iron meteorites were analyzed to search for nucleosynthetic isotope anomalies and to find evidence of formerly live 126Sn, which decays to 126Te with a half-life of 234,500 yr. None of the meteorites show evidence of mass dependent Te isotope fractionations larger than 2‰ for δ 126/128Te. Following internal normalization of the data to 125Te/ 128Te, the Te isotope ratios of all analyzed meteorites were found to be identical to a terrestrial standard, within uncertainties. This provides evidence that the regions of the solar disk that were sampled during accretion of the meteorite parent bodies were well mixed and homogeneous on a large scale, with respect to Te isotopes. The data acquired for bulk carbonaceous chondrites indicate that the initial 126Sn/ 118Sn ratio of the solar system was <4 × 10 -5, but this is dependent on the assumption that no redistribution of Sn and Te occurred since the start of the solar system. Five Archean sedimentary sulfides that display both mass dependent and mass-independent isotope effects for S yield internally normalized Te isotope data, which indicate that mass-independent Te isotope effects are absent. The mass dependent fractionations in these samples are constrained to be less than ˜1‰ for δ 126/128Te.

  14. Mass cytometry: technique for real time single cell multitarget immunoassay based on inductively coupled plasma time-of-flight mass spectrometry.

    Science.gov (United States)

    Bandura, Dmitry R; Baranov, Vladimir I; Ornatsky, Olga I; Antonov, Alexei; Kinach, Robert; Lou, Xudong; Pavlov, Serguei; Vorobiev, Sergey; Dick, John E; Tanner, Scott D

    2009-08-15

    A novel instrument for real time analysis of individual biological cells or other microparticles is described. The instrument is based on inductively coupled plasma time-of-flight mass spectrometry and comprises a three-aperture plasma-vacuum interface, a dc quadrupole turning optics for decoupling ions from neutral components, an rf quadrupole ion guide discriminating against low-mass dominant plasma ions, a point-to-parallel focusing dc quadrupole doublet, an orthogonal acceleration reflectron analyzer, a discrete dynode fast ion detector, and an 8-bit 1 GHz digitizer. A high spectrum generation frequency of 76.8 kHz provides capability for collecting multiple spectra from each particle-induced transient ion cloud, typically of 200-300 micros duration. It is shown that the transients can be resolved and characterized individually at a peak frequency of 1100 particles per second. Design considerations and optimization data are presented. The figures of merit of the instrument are measured under standard inductively coupled plasma (ICP) operating conditions ( 900 for m/z = 159, the sensitivity with a standard sample introduction system of >1.4 x 10(8) ion counts per second per mg L(-1) of Tb and an abundance sensitivity of (6 x 10(-4))-(1.4 x 10(-3)) (trailing and leading masses, respectively) are shown. The mass range (m/z = 125-215) and abundance sensitivity are sufficient for elemental immunoassay with up to 60 distinct available elemental tags. When 500) can be used, which provides >2.4 x 10(8) cps per mg L(-1) of Tb, at (1.5 x 10(-3))-(5.0 x 10(-3)) abundance sensitivity. The real-time simultaneous detection of multiple isotopes from individual 1.8 microm polystyrene beads labeled with lanthanides is shown. A real time single cell 20 antigen expression assay of model cell lines and leukemia patient samples immuno-labeled with lanthanide-tagged antibodies is presented.

  15. Automated Sample Preparation Platform for Mass Spectrometry-Based Plasma Proteomics and Biomarker Discovery

    Directory of Open Access Journals (Sweden)

    Vilém Guryča

    2014-03-01

    Full Text Available The identification of novel biomarkers from human plasma remains a critical need in order to develop and monitor drug therapies for nearly all disease areas. The discovery of novel plasma biomarkers is, however, significantly hampered by the complexity and dynamic range of proteins within plasma, as well as the inherent variability in composition from patient to patient. In addition, it is widely accepted that most soluble plasma biomarkers for diseases such as cancer will be represented by tissue leakage products, circulating in plasma at low levels. It is therefore necessary to find approaches with the prerequisite level of sensitivity in such a complex biological matrix. Strategies for fractionating the plasma proteome have been suggested, but improvements in sensitivity are often negated by the resultant process variability. Here we describe an approach using multidimensional chromatography and on-line protein derivatization, which allows for higher sensitivity, whilst minimizing the process variability. In order to evaluate this automated process fully, we demonstrate three levels of processing and compare sensitivity, throughput and reproducibility. We demonstrate that high sensitivity analysis of the human plasma proteome is possible down to the low ng/mL or even high pg/mL level with a high degree of technical reproducibility.

  16. Anomalous-plasmoid-ejection-induced secondary magnetic reconnection: modeling solar flares and coronal mass ejections by laser–plasma experiments

    Institute of Scientific and Technical Information of China (English)

    Quanli; Dong; Dawei; Yuan; Shoujun; Wang; Xun; Liu; Yutong; Li; Xiaoxuan; Lin; Huigang; Wei; Jiayong; Zhong; Shaoen; Jiang; Yongkun; Ding; Bobin; Jiang; Kai; Du; Yongjian; Tang; Mingyang; Yu; Xiantu; He; Neng; Hua; Zhanfeng; Qiao; Kuixi; Huang; Ming; Chen; Jianqiang; Zhu; Gang; Zhao; Zhengming; Sheng; Jie; Zhang

    2013-01-01

    The driving mechanism of solar flares and coronal mass ejections is a topic of ongoing debate, apart from the consensus that magnetic reconnection plays a key role during the impulsive process. While present solar research mostly depends on observations and theoretical models, laboratory experiments based on high-energy density facilities provide the third method for quantitatively comparing astrophysical observations and models with data achieved in experimental settings.In this article, we show laboratory modeling of solar flares and coronal mass ejections by constructing the magnetic reconnection system with two mutually approaching laser-produced plasmas circumfused of self-generated megagauss magnetic fields. Due to the Euler similarity between the laboratory and solar plasma systems, the present experiments demonstrate the morphological reproduction of flares and coronal mass ejections in solar observations in a scaled sense,and confirm the theory and model predictions about the current-sheet-born anomalous plasmoid as the initial stage of coronal mass ejections, and the behavior of moving-away plasmoid stretching the primary reconnected field lines into a secondary current sheet conjoined with two bright ridges identified as solar flares.

  17. Evidence of a role for fat-free body mass in modulation of plasma carotenoid concentrations in older men: studies with hydrodensitometry.

    Science.gov (United States)

    Zhu, Y I; Hsieh, W C; Parker, R S; Herraiz, L A; Haas, J D; Swanson, J E; Roe, D A

    1997-02-01

    We examined the relationship between body composition and changes in plasma carotenoid concentration in response to dietary carotenoid restriction or beta-carotene (betaC) supplementation in healthy older men. Subjects (mean age 65 y) were assigned randomly to supplement (30 mg betaC/d) or placebo groups, and all subjects consumed a standard low carotenoid basal diet plus 1.5 mg betaC/d as carrots. Body composition was measured at baseline by hydrodensitometry, and plasma carotenoids were measured at baseline and after 28 d of treatment by HPLC. Baseline plasma total carotenoid concentration was significantly and negatively correlated with body mass index (BMI) and fat-free mass (FFM) but not with fat mass, whereas baseline betaC concentration was negatively associated with all three variables. The increase in plasma betaC concentration in response to betaC supplementation was significantly and inversely correlated with BMI and FFM but not with fat mass. Likewise, the decline in plasma total carotenoid concentration in the placebo group was also significantly and inversely related to BMI and FFM but not to fat mass. Thus, FFM seems to be an important determinant of plasma carotenoid concentrations and to explain a substantial portion of the often-observed relationship between BMI and blood carotenoid levels. Fat-free mass seems to represent a dynamic reservoir that dampens short-term changes in plasma carotenoid concentrations during fluctuation in carotenoid intake.

  18. Quantification and confirmation of flunixin in equine plasma by liquid chromatography-quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Luo, Yi; Rudy, Jeffrey A; Uboh, Cornelius E; Soma, Lawrence R; Guan, Fuyu; Enright, James M; Tsang, Deborah S

    2004-03-05

    The method describes quantification and confirmation of flunixin in equine plasma by liquid chromatography-quadrupole time-of-flight mass spectrometry (LC/Q-TOF/MS/MS). Samples were screened by enzyme-linked immunosorbent assay (ELISA) and only those samples presumptively declared positive were subjected to quantification and confirmation for the presence of flunixin by this method. The method is also readily adaptable to instrumental screening for the analyte. Flunixin was recovered from plasma by liquid-liquid extraction (LLE). The sample was diluted with 2 ml saturated phosphate buffer (pH 3.10) prior to LLE. The dried extract was reconstituted in acetonitrile:water:formic acid (50:50:0.1, v/v/v) and subsequently analyzed on a Q-TOF tandem mass spectrometer (Micromass) operated under electrospray ionization positive ion mode. The concentration of flunixin was determined by the internal standard (IS) calibration method using the peak area ratio with clonixin as the IS. The limits of detection (LOD) and quantification (LOQ) for flunixin in equine plasma were 0.1 and 1 ng/ml, respectively, whereas the limit of confirmation (LOC) was 2.5 ng/ml. The qualifying ions for the identification of flunixin were m/z 297 [M+H](+), 279 (BP), 264, 259, 239 and those for clonixin (IS) were m/z 263 [M+H](+), 245 (BP) and 210. The measurement uncertainty about the result was 8.7%. The method is simple, sensitive, robust and reliably fast in the quantification and confirmation of flunixin in equine plasma. Application of this method will assist racing authorities in the enforcement of tolerance plasma concentration of flunixin in the racehorse on race day.

  19. Determination of suvorexant in human plasma using 96-well liquid-liquid extraction and HPLC with tandem mass spectrometric detection.

    Science.gov (United States)

    Breidinger, S A; Simpson, R C; Mangin, E; Woolf, E J

    2015-10-01

    A method, using liquid chromatography with tandem mass spectrometric detection (LC-MS/MS), was developed for the determination of suvorexant (MK-4305, Belsomra(®)), a selective dual orexin receptor antagonist for the treatment insomnia, in human plasma over the concentration range of 1-1000ng/mL. Stable isotope labeled (13)C(2)H3-suvorexant was used as an internal standard. The sample preparation procedure utilized liquid-liquid extraction, in the 96-well format, of a 100μL plasma sample with methyl t-butyl ether. The compounds were chromatographed under isocratic conditions on a Waters dC18 (50×2.1mm, 3μm) column with a mobile phase consisting of 30/70 (v/v %) 10mM ammonium formate, pH3/acetonitrile at a flow rate of 0.3mL/min. Multiple reaction monitoring of the precursor-to-product ion pairs for suvorexant (m/z 451→186) and (13)C(2)H3-suvorexant (m/z 455→190) on an Applied Biosystems API 4000 tandem mass spectrometer was used for quantitation. Intraday assay precision, assessed in six different lots of control plasma, was within 10% CV at all concentrations, while assay accuracy ranged from 95.6 to 105.0% of nominal. Quality control (QC) samples in plasma were stored at -20°C. Initial within day analysis of QCs after one freeze-thaw cycle showed accuracy within 9.5% of nominal with precision (CV) of 6.7% or less. The plasma QC samples were demonstrated to be stable for up to 25 months at -20°C. The method described has been used to support clinical studies during Phase I through III of clinical development.

  20. Investigation of lanthanum-strontium-cobalt ferrites using laser ablation inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Óvári, Mihály; Tarsoly, Gergely; Németh, Zoltán; Mihucz, Victor G.; Záray, Gyula

    2017-01-01

    In the present study, suitability of laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for characterization of the purity and homogeneity of lanthanum-strontium-cobalt ferrite (LSCF) ceramic microsamples with general formula La1 - xSrxFe0.025Co0.975O3 (0.00 ≤ x ≤ 0.50) was studied through determination of their Sr:La ratios as well as Sr content either in depth or line profiling mode. The Sr content of the LSCF samples expressed as weight percent ranged between 5.8% and 9.7% in the case of wet chemical ICP-MS analysis, while theoretical values varied from 5.5% to 9.4%. In the case of LA-ICP-MS, relative standard deviation of the La-normalized Sr intensities was sufficient to characterize the homogeneity of the studied samples. Major and trace element (Mn, Ni, Cu, Mg, Al, Ba) concentrations could be detected at medium resolution of the applied sector field ICP-MS instrument after microwave-assisted acid digestion. For depth and line profiling, a successful approach consisted of the normalization of intensities of Sr, Fe and Co with the corresponding La counts. For the determination of the elemental ratios of La and Sr, the methods involving LA were in good agreement with theoretical values by standardization to an in-house standard corresponding to the LSCF sample having the highest x value (i.e., 0.50) checked by wet chemical ICP-MS measurements. Thus, assessment of fine scale doping of synthesized perovskite type of microsamples could be achieved by the proposed LA-ICP-MS based on a novel calibration approach applying an in-house perovskite standard. Therefore, LA-ICP-MS can be recommended for quality control of perovskite-based products. In memoriam Attila Vértes (1934-2011), full professor of the Institute of Chemistry, Eötvös Loránd University, Budapest, Hungary.

  1. Evaluation of the analytical capability of NIR femtosecond laser ablation-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Hirata, Takafumi; Kon, Yoshiaki

    2008-03-01

    A laser ablation-inductively coupled plasma-mass spectrometric (LA-ICPMS) technique utilizing a titanium-sapphire (TiS) femtosecond laser (fs-laser) has been developed for elemental and isotopic analysis. The signal intensity profile, depth of the ablation pit and level of elemental fractionation were investigated in order to evaluate the analytical capability of the present fs-laser ablation-ICPMS technique. The signal intensity profile of (57)Fe, obtained from iron sulfide (FeS(2)), demonstrated that the resulting signal intensity of (57)Fe achieved by the fs-laser ablation was almost 4-times higher than that obtained by ArF excimer laser ablation under a similar energy fluence (5 J/cm(2)). In fs-laser ablation, there is no significant difference in a depth of the ablation pit between glass and zircon material, while in ArF laser ablation, the resulting crater depth on the zircon crystal was almost half the level than that obtained for glass material. Both the thermal-induced and particle size-related elemental fractionations, which have been thought to be main sources of analytical error in the LA-ICPMS analysis, were measured on a Harvard 91500 zircon crystal. The resulting fractionation indexes on the (206)Pb/(238)U (f(Pb/U)) and (238)U/(232)Th (f(U/Th)) ratios obtained by the present fs-laser ablation system were significantly smaller than those obtained by a conventional ArF excimer laser ablation system, demonstrative of smaller elemental fractionation. Using the present fs-laser ablation technique, the time profile of the signal intensity of (56)Fe and the isotopic ratios ((57)Fe/(54)Fe and (56)Fe/(54)Fe) have been measured on a natural pyrite (FeS(2)) sample. Repeatability in signal intensity of (56)Fe achieved by the fs-laser ablation system was significantly better than that obtained by ArF excimer laser ablation. Moreover, the resulting precision in (57)Fe/(54)Fe and (56)Fe/(54)Fe ratio measurements could be improved by the fs-laser ablation system

  2. Ultracentrifugation and inductively coupled plasma mass spectrometry for metal-protein equilibrium studies

    Science.gov (United States)

    Arnquist, Isaac J.; Holcombe, James A.

    2012-10-01

    The coupling of separation by preparative ultracentrifugation and metal detection by inductively coupled plasma mass spectrometry (ICP-MS) has been explored for metal-protein equilibrium determinations. This study characterizes the stoichiometry as well as apparent (Kapp) and intrinsic (Kint) binding affinities of the metal-protein association for a model protein. In particular, the affinity of Cu2 + for the high affinity binding site in bovine serum albumin (BSA) is determined. Once equilibrium is established between Cu2 + and BSA, preparative ultracentrifugation moves the metalloprotein away from the meniscus, leaving unbound equilibrium copper in the protein free solution. Since the initial (total) concentrations of purified BSA and Cu2 + can be determined, the free copper concentration at equilibrium can also be determined by taking a small aliquot above the sedimenting boundary for analysis using ICP-MS. This analysis allows for the determination of free Cu2 + ion, which is identical to the equilibrium concentration prior to ultracentrifugation. From these data Kapp and Kint were determined at two different conditions, 100 mM Tris(hydroxymethyl)aminomethane (Tris) at pH 9.53 and pH 7.93. log Kapp values of 17.6 and 14.6 were determined at pH 9.53 and pH 7.93, respectively. Furthermore, pH-independent log Kint values of - 1.43 and - 1.04 were determined at pH 9.53 and 7.93, respectively. While the log Kint at pH 9.53 was in good agreement with literature values obtained from alternative methods, Kint at pH 7.93 was about 2.5 × larger than previously reported. BSA undergoes a structural rearrangement between pH 7-9, and the generally accepted pH-dependency of protein tertiary structure may be responsible for the variations in the "intrinsic" binding constant. The Cu-BSA binding affinity was also monitored in 100 mM Tris 0.1% sodium dodecyl sulfate (SDS) solution at pH 7.93 in order to determine the effect of a denaturant on metal binding. Results for both log

  3. [Selenium determination in plasma/serum by inductively coupled plasma mass spectrometry (ICP-MS): comparison with graphite furnace atomic absorption spectrometry (GF-AAS)].

    Science.gov (United States)

    Janasik, Beata; Trzcinka-Ochocka, Małgorzata; Brodzka, Renata

    2011-01-01

    The present study was aimed at comparing two techniques of selenium (Se) determination in serum/plasma samples: inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption (GF-AAS). Blood samples were collected by venipuncture, using Venosafe closed blood sampling system. The samples were centrifuged. The measurements were performed by Elan DRC-e mass spectrometry, Perkin Elmer, SCIEX, USA and Unicam Solar 989 QZ atomic absorption spectrometry. Reference material, Clincheck Serum Control Level 1 (Recipe, Germany), was used to verify the determinations. The Laboratory participates in external quality control (G-EQUAS). Analytical parameters for both techniques are respectively: ICP-MS--precision 5.9%, limit of detection 0.19 microg/l, repeatability 5.5%, trueness 2.4%, bias 97.6%, GF-AAS--precision 8%, limit of detection 3.4 microg/l, repeatability 7.2%, trueness 6.8%, bias 93.2%. The benefits of the ICP-MS technique are high accuracy, low detection limits and the possibility of multi-element analysis.

  4. Comparing Theory and Experiment for Analyte Transport in the First Vacuum Stage of the Inductively Coupled Plasma Mass Spectrometer

    Science.gov (United States)

    Zachreson, Matthew R.

    The inductively coupled plasma mass spectrometer (ICP-MS) has been used in laboratories for many years. The majority of the improvements to the instrument have been done empirically through trial and error. A few fluid models have been made, which have given a general description of the flow through the mass spectrometer interface. However, due to long mean free path effects and other factors, it is very difficult to simulate the flow details well enough to predict how changing the interface design will change the formation of the ion beam. Towards this end, Spencer et al. developed FENIX, a direct simulation Monte Carlo algorithm capable of modeling this transitional flow through the mass spectrometer interface, the transitional flow from disorganized plasma to focused ion beam. Their previous work describes how FENIX simulates the neutral ion flow. While understanding the argon flow is essential to understanding the ICP-MS, the true goal is to improve its analyte detection capabilities. In this work, we develop a model for adding analyte to FENIX and compare it to previously collected experimental data. We also calculate how much ambipolar fields, plasma sheaths, and electron-ion recombination affect the ion beam formation. We find that behind the sampling interface there is no evidence of turbulent mixing. The behavior of the analyte seems to be described simply by convection and diffusion. Also, ambipolar field effects are small and do not significantly affect ion beam formation between the sampler and skimmer cones. We also find that the plasma sheath that forms around the sampling cone does not significantly affect the analyte flow downstream from the skimmer. However, it does thermally insulate the electrons from the sampling cone, which reduces ion-electron recombination. We also develop a model for electron-ion recombination. By comparing it to experimental data, we find that significant amounts of electron-ion recombination occurs just downstream from the

  5. Delay time embedding of mass loss avalanches in a fusion plasma-oriented sandpile model

    Science.gov (United States)

    Bowie, C. A.; Dendy, R. O.; Hole, M. J.

    2016-10-01

    The sandpile paradigm is widely used to model aspects of the phenomenology of magnetically confined fusion (MCF) plasmas, including enhanced confinement, edge pedestals and, potentially, the impulsive energy and particle release process known as ELMing. Here we identify new points of contact between ELMing and the systemwide avalanches in a sandpile. We compare the quantified response [Calderon et al., Phys. Plasmas 20, 042306 (2014)] to increased fuelling of the time sequence of edge localised mode events in a series of similar Joint European Torus plasmas with the response to increased fuelling of the time sequence of systemwide avalanches in a sandpile model [Chapman et al., Phys. Rev. Lett. 86, 2814 (2001)] that has well established links to MCF plasma phenomenology. Both the probability density functions of inter-event time intervals, and delay time embeddings of event time sequences, at different fuelling rates, show common features and point to shared underlying physics.

  6. Modified quadrupole mass analyzer RGA-100 for beam plasma research in forevacuum pressure range

    Energy Technology Data Exchange (ETDEWEB)

    Zolotukhin, D. B.; Tyunkov, A. V. [Tomsk State University of Control Systems and Radioelectronics, 40 Lenin Ave., Tomsk 634050 (Russian Federation); Yushkov, Yu. G., E-mail: yuyushkov@gmail.com [Tomsk State University of Control Systems and Radioelectronics, 40 Lenin Ave., Tomsk 634050 (Russian Federation); Tomsk Polytechnic University, 30 Lenin Ave., Tomsk 634050 (Russian Federation); Oks, E. M. [Tomsk State University of Control Systems and Radioelectronics, 40 Lenin Ave., Tomsk 634050 (Russian Federation); Institute of High Current Electronics SB RAS, 2/3, Akademichesky Ave., Tomsk 634055 (Russian Federation)

    2015-12-15

    The industrial quadrupole RGA-100 residual gas analyzer was modified for the research of electron beam-generated plasma at forevacuum pressure range. The standard ionizer of the RGA-100 was replaced by three electrode extracting unit. We made the optimization of operation parameters in order to provide the maximum values of measured currents of any ion species. The modified analyzer was successfully tested with beam plasma of argon, nitrogen, oxygen, and hydrocarbons.

  7. Bioimaging of metals and biomolecules in mouse heart by laser ablation inductively coupled plasma mass spectrometry and secondary ion mass spectrometry.

    Science.gov (United States)

    Becker, J Sabine; Breuer, Uwe; Hsieh, Hui-Fang; Osterholt, Tobias; Kumtabtim, Usarat; Wu, Bei; Matusch, Andreas; Caruso, Joseph A; Qin, Zhenyu

    2010-11-15

    Bioimaging mass spectrometric techniques allow direct mapping of metal and biomolecule distributions with high spatial resolution in biological tissue. In this study laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) was used for imaging of transition metals (Fe, Cu, Zn, Mn, and Ti), alkali and alkaline-earth metals (Na, K, Mg, and Ca, respectively), and selected nonmetals (such as C, P, and S) in native cryosections of mouse heart. The metal and nonmetal images clearly illustrated the shape and the anatomy of the samples. Zinc and copper were inhomogeneously distributed with average concentrations of 26 and 11 μg g(-1), respectively. Titanium and manganese were detected at concentrations reaching 1 and 2 μg g(-1), respectively. The highest regional metal concentration of 360 μg g(-1)was observed for iron in blood present in the lumen of the aorta. Secondary ion mass spectrometry (SIMS) as an elemental and biomolecular mass spectrometric technique was employed for imaging of Na, K, and selected biomolecules (e.g., phosphocholine, choline, cholesterol) in adjacent sections. Here, two different bioimaging techniques, LA-ICPMS and SIMS, were combined for the first time, yielding novel information on both elemental and biomolecular distributions.

  8. Detection of cervical cancer biomarker patterns in blood plasma and urine by differential scanning calorimetry and mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Nichola C Garbett

    Full Text Available Improved methods for the accurate identification of both the presence and severity of cervical intraepithelial neoplasia (CIN and extent of spread of invasive carcinomas of the cervix (IC are needed. Differential scanning calorimetry (DSC has recently been shown to detect specific changes in the thermal behavior of blood plasma proteins in several diseases. This methodology is being explored to provide a complementary approach for screening of cervical disease. The present study evaluated the utility of DSC in differentiating between healthy controls, increasing severity of CIN and early and advanced IC. Significant discrimination was apparent relative to the extent of disease with no clear effect of demographic factors such as age, ethnicity, smoking status and parity. Of most clinical relevance, there was strong differentiation of CIN from healthy controls and IC, and amongst patients with IC between FIGO Stage I and advanced cancer. The observed disease-specific changes in DSC profiles (thermograms were hypothesized to reflect differential expression of disease biomarkers that subsequently bound to and affected the thermal behavior of the most abundant plasma proteins. The effect of interacting biomarkers can be inferred from the modulation of thermograms but cannot be directly identified by DSC. To investigate the nature of the proposed interactions, mass spectrometry (MS analyses were employed. Quantitative assessment of the low molecular weight protein fragments of plasma and urine samples revealed a small list of peptides whose abundance was correlated with the extent of cervical disease, with the most striking plasma peptidome data supporting the interactome theory of peptide portioning to abundant plasma proteins. The combined DSC and MS approach in this study was successful in identifying unique biomarker signatures for cervical cancer and demonstrated the utility of DSC plasma profiles as a complementary diagnostic tool to evaluate

  9. Detection of cervical cancer biomarker patterns in blood plasma and urine by differential scanning calorimetry and mass spectrometry.

    Science.gov (United States)

    Garbett, Nichola C; Merchant, Michael L; Helm, C William; Jenson, Alfred B; Klein, Jon B; Chaires, Jonathan B

    2014-01-01

    Improved methods for the accurate identification of both the presence and severity of cervical intraepithelial neoplasia (CIN) and extent of spread of invasive carcinomas of the cervix (IC) are needed. Differential scanning calorimetry (DSC) has recently been shown to detect specific changes in the thermal behavior of blood plasma proteins in several diseases. This methodology is being explored to provide a complementary approach for screening of cervical disease. The present study evaluated the utility of DSC in differentiating between healthy controls, increasing severity of CIN and early and advanced IC. Significant discrimination was apparent relative to the extent of disease with no clear effect of demographic factors such as age, ethnicity, smoking status and parity. Of most clinical relevance, there was strong differentiation of CIN from healthy controls and IC, and amongst patients with IC between FIGO Stage I and advanced cancer. The observed disease-specific changes in DSC profiles (thermograms) were hypothesized to reflect differential expression of disease biomarkers that subsequently bound to and affected the thermal behavior of the most abundant plasma proteins. The effect of interacting biomarkers can be inferred from the modulation of thermograms but cannot be directly identified by DSC. To investigate the nature of the proposed interactions, mass spectrometry (MS) analyses were employed. Quantitative assessment of the low molecular weight protein fragments of plasma and urine samples revealed a small list of peptides whose abundance was correlated with the extent of cervical disease, with the most striking plasma peptidome data supporting the interactome theory of peptide portioning to abundant plasma proteins. The combined DSC and MS approach in this study was successful in identifying unique biomarker signatures for cervical cancer and demonstrated the utility of DSC plasma profiles as a complementary diagnostic tool to evaluate cervical cancer

  10. A simple and selective liquid chromatography- tandem mass spectrometry method for determination of ε-aminocaproic acid in human plasma

    Directory of Open Access Journals (Sweden)

    Ganesh S. Moorthy

    2015-07-01

    Full Text Available Understanding the clinical pharmacology of the antifibrinolytic drug epsilon-aminocaproic acid (EACA is critical for rational drug administration in children. The aim of this study is to develop a reliable assay for the determination of EACA in human plasma. We describe a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS assay for EACA in human plasma. Sample preparation involved plasma dilution (1:2040, followed by reversed-phase chromatographic separation and selective detection using tandem mass spectrometry. EACA had a linear range of 1 - 250 μg/mL. The intraday precision based on the standard deviation of replicates of quality control samples ranged from 4.7 to 10.4% and the accuracy ranged from 92-106%. The interday precision ranged from 4.6 to 9.8% and the accuracy ranged from 95-103%. Stability studies showed that EACA was stable during the conditions for sample preparation and storage. The described method is robust and successfully employed for clinical studies of EACA in children

  11. Simultaneous determination of piroxicam, meloxicam and tenoxicam in human plasma by liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Ji, Hye Young; Lee, Hye Won; Kim, Young Hoon; Jeong, Dong Won; Lee, Hye Suk

    2005-11-05

    A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the determination of piroxicam, meloxicam and tenoxicam in human plasma was developed. Piroxicam, meloxicam, tenoxicam and isoxicam (internal standard) were extracted from human plasma with ethyl acetate at acidic pH and analyzed on a Sunfire column with the mobile phase of methanol:ammonium formate (15 mM, pH 3.0) (60:40, v/v). The analytes were detected using a mass spectrometer, equipped with electrospray ion source. The instrument was set in the multiple-reaction-monitoring (MRM) mode. The standard curve was linear (r=1.000) over the concentration range of 0.50-200 ng/ml. The coefficient of variation (CV) and relative error (RE) for intra- and inter-assay statistics at three QC levels were 1.0-5.4% and -5.9 to 2.8%, respectively. The recoveries of piroxicam, meloxicam and tenoxicam ranged from 78.3 to 87.1%, with that of isoxicam being 59.7%. The lower limit of quantification for piroxicam, meloxicam and tenoxicam was 0.50 ng/ml using a 100 microl plasma sample. This method was successfully applied to a pharmacokinetic study of piroxicam after application of transdermal piroxicam patches to humans.

  12. Sensitive liquid chromatography-tandem mass spectrometry method for the simultaneous determination of paracetamol and guaifenesin in human plasma.

    Science.gov (United States)

    Chen, Xiaoyan; Huang, Jia; Kong, Zhang; Zhong, Dafang

    2005-03-25

    A rapid and sensitive method for the simultaneous determination of paracetamol and guaifenesin in human plasma was developed and validated, using high-performance liquid chromatographic separation with tandem mass spectrometric detection. After extracted from plasma samples by diethyl ether-dichloromethane (3:2, v/v), the analytes and internal standard osalmide were chromatographed on a C18 column. Detection was performed on a triple quadrupole tandem mass spectrometer by selected reaction monitoring (SRM) mode via atmospheric pressure chemical ionization (APCI). The method was linear in the concentration range of 0.05-20.0 microg/ml for paracetamol and 5.0-2000.0 ng/ml for guaifenesin. The intra- and inter-day precision was within 14% for both paracetamol and guaifenesin. The assay accuracy was within +/-2.4% for the analytes. This is the first assay method described for the simultaneous determination of paracetamol and guaifenesin in plasma using one chromatographic run. The method was successfully employed in a pharmacokinetic study after an oral administration of a multicomponent formulation, containing 650 mg paracetamol, 200 mg guaifenesin, 60 mg pseudoephedrine and 20 mg dextrorphan.

  13. Optimized ultra performance liquid chromatography tandem high resolution mass spectrometry method for the quantification of paraquat in plasma and urine.

    Science.gov (United States)

    Lu, Haihua; Yu, Jing; Wu, Linlin; Xing, Jingjing; Wang, Jun; Huang, Peipei; Zhang, Jinsong; Xiao, Hang; Gao, Rong

    2016-08-01

    A simple, sensitive and specific ultra performance liquid chromatography coupled to electrospray tandem high resolution mass spectrometry (UPLC-ESI-HRMS/MS) method has been developed and validated for quantification of paraquat in plasma and urine. The sample preparation was carried out by one-step protein precipitation with acetonitrile. The paraquat was separated with a HILIC column in 10min. Detection was performed using Q Exactive Orbitrap mass spectrometer by Targeted-MS/MS scan mode. Methodological parameters, such as ammonium formate concentration, formic acid concentration, spray voltage, capillary temperature, heater temperature and normalized collision energy were optimized to achieve the highest sensitivity. The calibration curve was linear over the concentration range of LOQ-1000ng/mL. LOD was 0.1 and 0.3ng/mL, LOQ was 0.3 and 0.8ng/mL for urine and plasma, respectively. The intra- and inter-day precisions were paraquat concentration in plasma samples with hemoperfusion from 5 suspected paraquat poisoning patients.

  14. Mass number identification by Alfvén wave diagnostics in hydrogen and helium plasmas in TCABR

    Energy Technology Data Exchange (ETDEWEB)

    Puglia, P.G.P.; Elfimov, A.G., E-mail: elfimov@if.usp.br; Andriati, A.V.; Galvão, R.M.O.; Guimarães-Filho, Z.O.; Ronchi, G.; Ruchko, L.F.

    2016-03-11

    The mass number is obtained through the identification of the Global Alfvén (GA) wave resonances in ohmic plasma discharges in the TCABR tokamak. By comparing hydrogen and helium discharges, the composition of carbon, oxygen, and iron impurities is determined. The non-perturbative Alfvén diagnostic is used that is based on the excitation of GA waves by an external antenna fed by a low power generator, in the frequency band swept just below the minimum of the Alfvén wave continuum. Odd or even toroidal modes are excited by selecting the current phase in the two antenna modules separated by 180 degrees in the toroidal direction. The density profile, determined from cross analysis of reflectometer and interferometer data, shows impurity accumulation in the plasma core. - Highlights: • A non-perturbative Alfvén diagnostic is used to find the mass number in ohmic discharges in TCABR tokamak. • Global Alfvén waves are excited by an external antenna fed by a low power generator at the minimum of the Alfvén continuum. • Comparing hydrogen and helium discharges, the composition of carbon, oxygen and iron impurities is determined. • The density profile defined reflectometer and interferometer data shows impurity accumulation in the plasma core.

  15. Development and validation of liquid chromatography-Mass spectrometry method for the estimation of rifampicin in plasma

    Directory of Open Access Journals (Sweden)

    J S Patil

    2011-01-01

    Full Text Available A selective, rapid and sensitive liquid chromatography-mass spectrometry method was developed for the quantitative estimation of rifampicin in plasma. With phenacetin as internal standard, sample pretreatment involved a one-step extraction with ethyl acetate from plasma. The sample was analyzed using methanol: 2mM ammonium acetate: 80:20 v/v as mobile phase. Chromatographic separation was achieved on a BDS Hypersil Gold C 18 column which was followed by detection with mass spectrometry. Linear calibration curves were obtained in the concentration range of 5.021-1008.315 ng/ml. The inter- and intra-day accuracy values were below 15% at all quality control levels. Percent recoveries for rifampicin at high, middle and low quality control samples was obtained 55.15, 48.65 and 49.62%, respectively and for internal standard was 60.22%. Rifampicin was found stable through all validation parameters. Developed method was found to be simple, precise, accurate and rapid for estimation of rifampicin in plasma. Thus, the method can be employed for routine pharmacokinetic and bioequivalence studies.

  16. Quantitative determination of oxytocin receptor antagonist atosiban in rat plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Kannan, Vivekanandan; Gadamsetty, Deepak; Rose, Madhankumar; Maria, Stella; Mustafa, Imran; Khedkar, Anand; Dave, Nitesh; Arumugam, Muruganandam; Iyer, Harish

    2010-05-01

    A kinetic study of atosiban was conducted following repeated intravenous administration in Wistar rats. Sample analysis was performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) following full validation of an in-house method. Eptifibatide, a cyclic peptide, was used as an internal standard (IS). The analyte and internal standard were extracted using solid phase extraction (SPE) method. Chromatographic separation was carried out using an ACE C18 5 microm 50 mm x 4.6 mm column with gradient elution. Mass spectrometric detection was performed using TSQ Quantum ultra AM. The lower limit of quantification was 0.01 microg/ml when 100 microl rat plasma was used. Plasma concentrations of atosiban were measured at 0 (pre-dose), 2, 15, 30, 45, 60, 120 min at the dosage levels of 0.125 mg/kg (low dose), 0.250 mg/kg (mid dose), and 0.500 mg/kg (high dose), respectively. Atosiban plasma concentration measured at Day 1 showed mean peak atosiban concentration (C(max)) 0.40, 0.57, 1.95 microg/ml for low, mid and high dose treated animals and mean peak concentration on Day 28 was 0.41, 0.88, 1.31microg/ml on Day 28 for low, mid and high dose treated animals.

  17. Mass spectrometry of positive ions and neutral species in the effluent of an atmospheric pressure plasma with hexamethyldisiloxane and oxygen

    Science.gov (United States)

    Benedikt, J.; Ellerweg, D.; Schneider, S.; Rügner, K.; R, Reuter; Kersten, H.; Benter, T.

    2013-11-01

    The effluent of a non-equilibrium atmospheric pressure plasma jet in He with admixture of hexamethyldisiloxane (HMDSO) and O2 has been investigated by means of molecular beam mass spectrometry. Positive ions and neutral plasma chemistry products have been detected and their possible role in the deposition of good-quality SiO2 films is discussed. Positive ion spectra reveal the presence of protonated water clusters and H+ : HMDSO and H3O+ : HMDSO ions. These ions are most probably produced by photoionization. This is corroborated by optical emission spectroscopy data obtained in the wavelength range of 50-300 nm, where helium excimer continuum emission centred around 84 nm has been observed. No ion driven polymerization products of HMDSO have been detected. Measurements of neutral species have allowed the quantification of the HMDSO depletion and absolute densities of trimethylsilanol and pentamethyldisiloxane. Two neutral polymerization products have been observed as well. The results indicate that the Si-O bond of HMDSO is preferentially broken. Additionally, the mass balance of plasma chemistry products is discussed.

  18. Liquid chromatography-tandem mass spectrometric assay for the cyclin-dependent kinase inhibitor AT7519 in mouse plasma.

    Science.gov (United States)

    Dolman, M Emmy M; den Hartog, Ilona J M; Molenaar, Jan J; Schellens, Jan H M; Beijnen, Jos H; Sparidans, Rolf W

    2014-01-01

    A quantitative bioanalytical liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay for the cyclin-dependent kinase inhibitor AT7519 in mouse plasma was developed and validated. Plasma samples were pre-treated using protein precipitation with acetonitrile containing rucaparib as internal standard. After dilution with water, the extract was directly injected into the reversed-phase LC system. The eluate was transferred into the electrospray interface with positive ionization and the analyte was detected in the selected reaction monitoring mode of a triple quadrupole mass spectrometer. The assay was validated in a 5-10,000ng/ml calibration range using double logarithmic calibration, 5ng/ml was the lower limit of quantification. Within day precisions (n=6) were 2.9-5.6%, between day (3 days; n=18) precisions 3.2-7.2%. Accuracies were between 95.9 and 99.0% for the whole calibration range. The drug was stable under all relevant analytical conditions. Finally, the assay was successfully used to determine plasma pharmacokinetics after intraperitoneal administration of AT7519 in mice with neuroblastoma xenografts. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Worsening diastolic function is associated with elevated fasting plasma glucose and increased left ventricular mass in a supra-additive fashion in an elderly, healthy, Swedish population

    DEFF Research Database (Denmark)

    Pareek, Manan; Nielsen, Mette Lundgren; Gerke, Oke;

    2015-01-01

    AIMS: To examine whether increasing fasting plasma glucose (FPG) levels were associated with worsening left ventricular (LV) diastolic function, independently of LV mass index (LVMI) in elderly, otherwise healthy subjects. METHODS AND RESULTS: We tested cross-sectional associations between...

  20. High spatial resolution analysis of Pb and U isotopes for geochronology by laser ablation multi-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS)

    National Research Council Canada - National Science Library

    Bühn, Bernhard; Pimentel, Márcio M; Matteini, Massimo; Dantas, Elton L

    2009-01-01

    ...), are widely used to decipher geological processes. A new method developed in the last couple of years, the laser ablation multi-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS...

  1. Quantitative Metabolite Profiling of an Amino Group Containing Pharmaceutical in Human Plasma via Precolumn Derivatization and High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry.

    Science.gov (United States)

    Li, Sanwang; Klencsár, Balázs; Balcaen, Lieve; Cuyckens, Filip; Lynen, Frederic; Vanhaecke, Frank

    2017-02-07

    Quantitative determination of the candidate drug molecule and its metabolites in biofluids and tissues is an inevitable step in the development of new pharmaceuticals. Because of the time-consuming and expensive nature of the current standard technique for quantitative metabolite profiling, i.e., radiolabeling followed by high-performance liquid chromatography (HPLC) with radiodetection, the development of alternative methodologies is of great interest. In this work, a simple, fast, sensitive, and accurate method for the quantitative metabolite profiling of an amino group containing drug (levothyroxine) and its metabolites in human plasma, based on precolumn derivatization followed by HPLC-inductively coupled plasma mass spectrometry (ICPMS), was developed and validated. To introduce a suitable "heteroelement" (defined here as an element that is detectable with ICPMS), an inexpensive and commercially available reagent, tetrabromophthalic anhydride (TBPA) was used for the derivatization of free NH2-groups. The presence of a known number of I atoms in both the drug molecule and its metabolites enabled a cross-validation of the newly developed derivatization procedure and quantification based on monitoring of the introduced Br. The formation of the derivatives was quantitative, providing a 4:1 stoichiometric Br/NH2 ratio. The derivatives were separated via reversed-phase HPLC with gradient elution. Bromine was determined via ICPMS at a mass-to-charge ratio of 79 using H2 as a reaction gas to ensure interference-free detection, and iodine was determined at a mass-to-charge ratio of 127 for cross-validation purposes. The method developed shows a fit-for-purpose accuracy (recovery between 85% and 115%) and precision (repeatability <15% RSD). The limit of quantification (LoQ) for Br was approximately 100 μg/L.

  2. Acute strength exercise and the involvement of small or large muscle mass on plasma brain-derived neurotrophic factor levels

    Directory of Open Access Journals (Sweden)

    Paulo Roberto Correia

    2010-01-01

    Full Text Available OBJECTIVE: Blood neurotrophins, such as the brain-derived neurotrophic factor, are considered to be of great importance in mediating the benefits of physical exercise. In this study, the effect of acute strength exercise and the involvement of small versus large muscle mass on the levels of plasma brain-derived neurotrophic factor were evaluated in healthy individuals. METHODS: The concentric strengths of knee (large and elbow (small flexor and extensor muscles were measured on two separate days. Venous blood samples were obtained from 16 healthy subjects before and after exercise. RESULTS: The levels of brain-derived neurotrophic factor in the plasma did not significantly increase after both arm and leg exercise. There was no significant difference in the plasma levels of the brain-derived neurotrophic factor in the arms and legs. CONCLUSION: The present results demonstrate that acute strength exercise does not induce significant alterations in the levels of brain-derived neurotrophic factor plasma concentrations in healthy individuals. Considering that its levels may be affected by various factors, such as exercise, these findings suggest that the type of exercise program may be a decisive factor in altering peripheral brain-derived neurotrophic factor.

  3. Fast determination of paraquat in plasma and urine samples by solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gao, Lina; Liu, Junting; Wang, Chunyuan; Liu, Guojie; Niu, Xiaodong; Shu, Cuixia; Zhu, Juan

    2014-01-01

    A simple, sensitive and reliable gas chromatographic-mass spectrometric method (GC-MS) for quantifying paraquat concentration in biological samples has been developed, using ethyl paraquat as an internal standard. The method involved the procedures of sodium borohydride-nickel chloride (NaBH4-NiCl2) reduction and solid-phase microextraction (SPME) of the perhydrogenated products. GC-MS was used to identify and quantify the analytes in selected ion monitoring (SIM) mode. Under the optimal conditions, recoveries in plasma and urine samples were 94.00-99.85% and 95.00-100.34%, respectively. Excellent sample clean-up was observed and good linearities (r=0.9982 for plasma sample and 0.9987 for urine sample) were obtained in the range of 0.1-50μg/mL. The limits of detection (S/N=3) were 0.01μg/mL in plasma and urine samples. The intra-day precision was less than 8.43%, 4.19% (n=3), and inter-day precision was less than 10.90%, 10.49% (n=5) for plasma and urine samples, respectively. This method was successfully applied to the analysis of the biological samples collected from a victim who died as a result of ingestion of paraquat.

  4. Mass fragmentographic assay of nanogram amounts of the antidepressant drug mianserin hydrochloride (Org GB 94) in human plasma.

    Science.gov (United States)

    de Ridder, J J; Koppens, P C; van Hal, H J

    1977-05-01

    For the assay of the antidepressant compound mianserin hydrochloride (Org GB 94) in human plasma, a mass fragmentographic method, using the deuterated analogue as internal standard and a high-performance liquid chromatographie sample clean-up procedure has been developed. The assay specifications obtained are a lower limit for reliable measurements of 1 ng/ml, and accuracy of ca. 0.01 ng/ml, a precision of 6--7% and a capacity of about 60 samples per day. The applicability of the assay method is illustrated by measurements of single-dose and steady-state plasma levels in clinical experiments, demonstrating the possibility of monitoring plasma levels during at least 24 h after a single dose of 15 mg of Org GB 94. The mean steady-state plasma levels after a daily dose of 3 X 20 mg of Org GB 94 appeared to be remarkably constant with time: 38, 36 and 34 ng/ml after 2, 4, and 6 weeks of treatment of 18 depressed patients.

  5. Determination of salbutamol in human plasma and urine using liquid chromatography coupled to tandem mass spectrometry and its pharmacokinetic study.

    Science.gov (United States)

    Zhang, Dujuan; Teng, Yanni; Chen, Keguang; Liu, Sha; Wei, Chunmin; Wang, Benjie; Yuan, Guiyan; Zhang, Rui; Liu, Xiaoyan; Guo, Ruichen

    2012-10-01

    A sensitive and selective liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) was developed and validated for the determination of salbutamol in human plasma and urine, and successfully applied to the pharmacokinetic study of salbutamol in Chinese healthy volunteers after inhalation of salbutamol sulfate aerosol. Salbutamol and the internal standard (IS) acetaminophen in plasma and urine were extracted with ethyl acetate, separated on a C(18) reversed-phase column, eluted with mobile phase of acetonitrile-ammonium acetate (5 m m; 30:70, v/v), ionized by positive ion pneumatically assisted electrospray and detected in the multi-reaction monitoring mode using precursor → product ions of m/z 240.2 → 148.1 for salbutamol and 152 → 110 for the IS. The lower limits of quantitation of salbutamol in human plasma and urine by this method were 0.02 and 1 ng/mL, respectively. The specificity, matrix effect, recovery, sensitivity, linearity, accuracy, precision and several stabilities were validated for salbutamol in human plasma and urine. In conclusion, the validation results showed that this method is robust, specific and sensitive, and can successfully fulfill the requirement of clinical pharmacokinetic study of salbutamol in healthy Chinese volunteers.

  6. Liquid chromatography–tandem mass spectrometry analysis of free and esterified fatty acid N-acyl ethanolamines in plasma and blood cells

    NARCIS (Netherlands)

    Balvers, M.G.J.; Wortelboer, H.M.; Witkamp, R.F.; Verhoeckx, K.C.M.

    2013-01-01

    The origin of N-acyl ethanolamides (NAEs) in plasma is not well understood, and it is possible that NAEs are present in plasma in esterified form. To test this hypothesis, a new and sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the quantif

  7. Determination of rutin in rat plasma by ultra performance liquid chromatography tandem mass spectrometry and application to pharmacokinetic study.

    Science.gov (United States)

    Chen, Mengchun; Zhang, Xiaoqian; Wang, Hao; Lin, Baoli; Wang, Shuanghu; Hu, Guoxin

    2015-04-01

    A sensitive and rapid ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) method for the determination of rutin in rat plasma was developed and validated. After addition of tolbutamide as internal standard (IS), protein precipitation by acetonitrile was used as sample preparation. The chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm particle size), using acetonitrile-0.1% formic acid as the mobile phase with gradient elution, delivered at a flow-rate of 0.4 mL/min. Mass spectrometric analysis was performed using a XEVO TQD mass spectrometer coupled with an electro-spray ionization (ESI) source in the positive ion mode. The MRM transitions of m/z 610.91→302.98 and m/z 271.2→155.1 were used to quantify for rutin and tolbutamide, respectively. This assay method has been fully validated in terms of specificity, linearity, recovery and matrix effect, accuracy, precision and stability. Calibration curves were linear in the concentration ranges of 25-2000 ng/mL for rutin. Only 3 min was needed for an analytical run. This developed method was successfully used for determination of rutin in rat plasma for pharmacokinetic study.

  8. Improving low-level plasma protein mass spectrometry-based detection for candidate biomarker discovery and validation

    Energy Technology Data Exchange (ETDEWEB)

    Page, Jason S.; Kelly, Ryan T.; Camp, David G.; Smith, Richard D.

    2008-09-01

    Methods. To improve the detection of low abundance protein candidate biomarker discovery and validation, particularly in complex biological fluids such as blood plasma, increased sensitivity is desired using mass spectrometry (MS)-based instrumentation. A key current limitation on the sensitivity of electrospray ionization (ESI) MS is due to the fact that many sample molecules in solution are never ionized, and the vast majority of the ions that are created are lost during transmission from atmospheric pressure to the low pressure region of the mass analyzer. Two key technologies, multi-nanoelectrospray emitters and the electrodynamic ion funnel have recently been developed and refined at Pacific Northwest National Laboratory (PNNL) to greatly improve the ionization and transmission efficiency of ESI MS based analyses. Multi-emitter based ESI enables the flow from a single source (typically a liquid chromatography [LC] column) to be divided among an array of emitters (Figure 1). The flow rate delivered to each emitter is thus reduced, allowing the well-documented benefits of nanoelectrospray 1 for both sensitivity and quantitation to be realized for higher flow rate separations. To complement the increased ionization efficiency afforded by multi-ESI, tandem electrodynamic ion funnels have also been developed at PNNL, and shown to greatly improve ion transmission efficiency in the ion source interface.2, 3 These technologies have been integrated into a triple quadrupole mass spectrometer for multiple reaction monitoring (MRM) of probable biomarker candidates in blood plasma and show promise for the identification of new species even at low level concentrations.

  9. Maternal plasma n-3 and n-6 polyunsaturated fatty acid concentrations during pregnancy and subcutaneous fat mass in infancy

    Science.gov (United States)

    Jelena Vidakovic, Aleksandra; Santos, Susana; Williams, Michelle A.; Duijts, Liesbeth; Hofman, Albert; Demmelmair, Hans; Koletzko, Berthold; Jaddoe, Vincent WV; Gaillard, Romy

    2017-01-01

    Objective We examined the associations of maternal plasma n-3 and n-6 PUFA concentrations during pregnancy with infant subcutaneous fat. Methods In a population-based prospective cohort study among 904 mothers and their infants, we measured maternal plasma n-3 and n-6 PUFA concentrations at mid-pregnancy. Body mass index, total subcutaneous fat and central-to-total subcutaneous fat ratio were calculated at 1.5, 6 and 24 months. Results Maternal n-3 PUFA levels were not consistently associated with infant body mass index or total subcutaneous fat. Higher maternal total n-3 PUFA levels, and specifically eicosapentaenoic acid (EPA), docosapentaenoic acid (DPA) and docosahexaenoic acid (DHA), were associated with higher central-to-total subcutaneous fat ratio at 1.5 months, whereas higher maternal total n-3 PUFA levels were associated with lower central-to-total subcutaneous fat ratio at 6 months (all p-values<0.05). These associations were not present at 24 months. Maternal n-6 PUFA levels were not consistently associated with infant subcutaneous fat. A higher n-6/n-3 ratio was associated with lower central-to-total subcutaneous fat ratio at 1.5 months only (p-value<0.05). Conclusions Maternal n-3 PUFA levels during pregnancy may have transient effects on infant subcutaneous fat. Further studies are needed to assess the effects of maternal PUFA concentrations on fat mass development during early infancy. PMID:27356181

  10. A Supercritical Fluid Chromatography/Tandem Mass Spectrometry Method for the Simultaneous Quantification of Metformin and Gliclazide in Human Plasma

    Science.gov (United States)

    Agrawal, Y. K.; Gogoi, P. J.; Manna, K.; Bhatt, H. G.; Jain, V. K.

    2010-01-01

    Present study reports the development and validation of a simultaneous estimation of metformin and gliclazide in human plasma using supercritical fluid chromatography followed by tandem mass spectrometry. Acetonitrile:water (80:20) mixture was used as a mobile phase along with liquid CO2 in supercritical fluid chromatography and phenformin as an internal standard. The modified plasma samples were analyzed by electro-spray ionization method in selective reaction monitoring mode in tandem mass spectrometry. Supercritical fluid chromatographic separation was performed using nucleosil C18 containing column as a stationary phase. The separated products were identified by characteristic peaks and specific fragments peaks in tandem mass spectrometry as m/z 130 to 86 for metformin, m/z 324 to 110 for gliclazide and m/z 206 to 105 for phenformin. The present method was found linear in the concentration ranges of 6.0-3550 ng/ml and 7.5-7500 ng/ml for metformin and gliclazide, respectively. Pharmacokinetic study was performed after an oral administration of dispersible tablets containing 500 mg of metformin and 80 mg of gliclazide using same techniques. PMID:20582190

  11. Ultracentrifugation and inductively coupled plasma mass spectrometry for metal-protein equilibrium studies

    Energy Technology Data Exchange (ETDEWEB)

    Arnquist, Isaac J.; Holcombe, James A., E-mail: holcombe@mail.utexas.edu

    2012-10-15

    The coupling of separation by preparative ultracentrifugation and metal detection by inductively coupled plasma mass spectrometry (ICP-MS) has been explored for metal-protein equilibrium determinations. This study characterizes the stoichiometry as well as apparent (K{sub app}) and intrinsic (K{sub int}) binding affinities of the metal-protein association for a model protein. In particular, the affinity of Cu{sup 2+} for the high affinity binding site in bovine serum albumin (BSA) is determined. Once equilibrium is established between Cu{sup 2+} and BSA, preparative ultracentrifugation moves the metalloprotein away from the meniscus, leaving unbound equilibrium copper in the protein free solution. Since the initial (total) concentrations of purified BSA and Cu{sup 2+} can be determined, the free copper concentration at equilibrium can also be determined by taking a small aliquot above the sedimenting boundary for analysis using ICP-MS. This analysis allows for the determination of free Cu{sup 2+} ion, which is identical to the equilibrium concentration prior to ultracentrifugation. From these data K{sub app} and K{sub int} were determined at two different conditions, 100 mM Tris(hydroxymethyl)aminomethane (Tris) at pH 9.53 and pH 7.93. log K{sub app} values of 17.6 and 14.6 were determined at pH 9.53 and pH 7.93, respectively. Furthermore, pH-independent log K{sub int} values of - 1.43 and - 1.04 were determined at pH 9.53 and 7.93, respectively. While the log K{sub int} at pH 9.53 was in good agreement with literature values obtained from alternative methods, K{sub int} at pH 7.93 was about 2.5 Multiplication-Sign larger than previously reported. BSA undergoes a structural rearrangement between pH 7-9, and the generally accepted pH-dependency of protein tertiary structure may be responsible for the variations in the 'intrinsic' binding constant. The Cu-BSA binding affinity was also monitored in 100 mM Tris 0.1% sodium dodecyl sulfate (SDS) solution at p

  12. Langmuir Probe and Mass Spectroscopic Measurements in Inductively Coupled CF4 Plasmas

    Science.gov (United States)

    Rao, M. V. V. S.; Sharma, Surendra; Cruden, B. A.; Meyyappan, M.

    2001-01-01

    Abstract Electron and ion energy distribution functions and other plasma parameters such as plasma potential (V(sub p)) , electron temperature (T(sub e)), and electron and ion number densities (n (sub e) and n(sub i)) in low pressure CF4 plasmas have been measured. The experiments were conducted in a GEC cell using an inductively coupled plasma (ICP) device powered by a 13.56 MHz radio-frequency (rf) power source. The measurements were made at 300 W of input rf power at 10, 30 and 50 mTorr gas pressures. Langmuir probe measurements suggest that n(sub e), n(sub i) and V(sub p) remain constant over 60% of the central electrode area, beyond which they decrease. Within the limits of experimental error (+/- 0.25 eV), T(sub e) remains nearly constant over the electrode area. T(sub e) and V(sub p) increase with a decrease in pressure. n(sub e) and n(sub i) are not affected as significantly as T(sub e) or V(sub p) by variation in the gas pressure. The electron energy distribution function (EEDF) measurements indicate a highly non-Maxwellian plasma. CF3+ is the most dominant ion product of the plasma, followed by CF2+ and CF+. The concentrations of CF2+ and CF+ are much larger than that is possible from direct electron impact ionization of the parent gas. The cross-section data suggest that the direct electron impact ionization of fragment neutrals and negative ion production by electron attachment may be responsible for increase of the minor ions.

  13. {sup 252}Cf plasma desorption and laser desorption mass spectrometry for the determination of molecular weight distribution of coal derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, B.R.; Bartle, K.D.; Ross, A.B.; Herod, A.A.; Kandiyoti, R.; Larsen, J.W. [University of Leeds, Leeds (United Kingdom). School of Chemistry

    1999-11-01

    A detailed knowledge of the molecular mass (MM) distribution in coal and its derived products is essential for a fundamental understanding of coal structure, and of the processes occurring during coal conversion. Fractionation using size exclusion chromatography (s.e.c.) using N-methyl-2-pyrrolidinone as the mobile phase has been applied to such materials and has provided improved MM distributions. Absolute calibration has been provided using matrix assisted laser desorption ionisation mass spectrometry (MAl.d.I.-m.s.). An alternative method of volatilising and ionising large molecules for mass spectrometry (m.s.) is {sup 252}Cf plasma desorption ({sup 252}Cf p.d.-m.s.). This involves the use of energetic fission fragments from the decay of {sup 252}Cf and produces mass spectra consisting predominantly of molecular ions from a range of polymers and biomolecules. This has been used by other workers to determine the molecular weight distribution of heavy distillation residues obtained from coal liquefaction processes either unfractionated or fractionated into broad fractions. Generally, a good agreement was obtained between values of MM determined by {sup 252}Cf p.d.-m.s. and s.e.c. A comparison is reported of MM distribution determined by {sup 252}Cf p.d.-m.s. and laser desorption mass spectrometry (l.d.-m.s.) for narrower fractions separated by s.e.c. from a coal tar pitch. 19 refs., 4 figs., 1 tab.

  14. Determination of talniflumate and niflumic acid in human plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Kang, Wonku; Kim, Kibum

    2009-04-01

    A simple and rapid quantification method was developed for determining both talniflumate and niflumic acid in human plasma. After simple protein precipitation with acetonitrile, the analytes were chromatographed on a reversed-phase C(18) column and detected by LC/MS/MS with electrospray ionization. The assay accuracy and precision were within the FDA guidance for the analytical method validation. This method was used to measure the plasma concentrations of both compounds from healthy subjects after a single oral dose of talniflumate, 740 mg.

  15. Reconstruction of energy and angle distribution function of surface-emitted negative ions in hydrogen plasmas using mass spectrometry

    Science.gov (United States)

    Kogut, D.; Achkasov, K.; Dubois, J. P. J.; Moussaoui, R.; Faure, J. B.; Layet, J. M.; Simonin, A.; Cartry, G.

    2017-04-01

    A new method involving mass spectrometry and modeling is described in this work, which may highlight the production mechanisms of negative ions (NIs) on surface in low pressure plasmas. Positive hydrogen ions from plasma impact a sample which is biased negatively with respect to the plasma potential. NIs are produced on the surface through the ionization of sputtered and backscattered particles and detected according to their energy and mass by a mass spectrometer (MS) placed in front of the sample. The shape of the measured negative-ion energy distribution function (NIEDF) strongly differs from the NIEDF of the ions emitted by the sample because of the limited acceptance angle of the MS. The reconstruction method proposed here allows to compute the distribution function in energy and angle (NIEADF) of the NIs emitted by the sample based on the NIEDF measurements at different tilt angles of the sample. The reconstruction algorithm does not depend on the NI surface production mechanism, so it can be applied to any type of surface and/or NI. The NIEADFs for highly oriented pyrolitic graphite (HOPG) and gadolinium (low work-function metal) are presented and compared with the SRIM modeling. HOPG and Gd show comparable integrated NI yields, however the key differences in mechanisms of NI production can be identified. While for Gd the major process is backscattering of ions with the peak of NIEDF at 36 eV, in case of HOPG the sputtering contribution due to adsorbed H on the surface is also important and the NIEDF peak is found at 5 eV.

  16. Differential Effects of Military Training on Fat-Free Mass and Plasma Amino Acid Adaptations in Men and Women

    Directory of Open Access Journals (Sweden)

    James P. McClung

    2012-12-01

    Full Text Available Fat-free mass (FFM adaptations to physical training may differ between sexes based on disparities in fitness level, dietary intake, and levels of plasma amino acids (AA. This investigation aimed to determine FFM and plasma AA responses to military training, examine whether adaptations differ between male and female recruits, and explore potential associations between FFM and AA responses to training. Body composition and plasma AA levels were assessed in US Army recruits (n = 209, 118 males, 91 females before (baseline and every three weeks during basic combat training (BCT, a 10-week military training course. Body weight decreased in men but remained stable in women during BCT (sex-by-time interaction, P < 0.05. Fifty-eight percent of recruits gained FFM during BCT, with more (P < 0.05 females (88% gaining FFM than males (36%. Total plasma AA increased (P < 0.05 during BCT, with greater (P < 0.05 increases observed in females (17% then in males (4%. Essential amino acids (EAA and branched-chain amino acids (BCAA were increased (P < 0.05 in females but did not change in males (sex-by-time interaction, P < 0.05. Independent of sex, changes in EAA (r = 0.34 and BCAA (r = 0.27 from baseline were associated with changes in FFM (P < 0.05; greater (P < 0.05 increases in AA concentrations were observed for those who gained FFM. Increases in FFM and plasma AA suggest that BCT elicits a more pronounced anabolic response in women compared to men, which may reflect sex-specific differences in the relative intensity of the combined training and physiological stimulus associated with BCT.

  17. Quantification of Warfarin in Dried Rat Plasma Spots by High-Performance Liquid Chromatography with Tandem Mass Spectrometry

    Science.gov (United States)

    2016-01-01

    This paper presents the development and validation of a novel method for quantification of the oral anticoagulant drug warfarin in dried plasma spots (DPS) by high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS). Blood plasma was chosen as a biological fluid to preclude the influence of the hematocrit on the results of the analysis. A 30 μL sample of rat plasma was placed onto Whatman 903 Protein Saver Card and was allowed to dry. A single DPS is sufficient for preparing eight 3.2 mm discs, each containing approximately 1.5–1.6 μL of plasma. Warfarin extraction from one 3.2 mm disc was carried out by adding 200 μL of the acetonitrile : water mixture (1 : 1, v/v) containing 10 mM NH4COOH (pH 4.0), with incubation on a shaker at 1000 rpm for 1 h at 25°C. After chromatographic separation, warfarin and coumachlor (an internal standard) were measured using negative-ion multiple-reaction monitoring with ion transitions m/z 307 → 161 for warfarin and m/z 341 → 161 for the internal standard. The working range of this method is 10–10,000 ng/mL. Within this range, intra- and interday variability of precision and accuracy was <13% and recovery was 82–99%. The results indicate that the new method requires only small plasma samples and may be useful for pharmacokinetic research on warfarin. PMID:28058133

  18. [Determination of 10 sedative-hypnotics in human plasma using pulse splitless injection technique and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Chang, Qing; Ma, Hongying; Wang, Fangjie; Ou, Honglian; Zou, Ming

    2011-11-01

    A simple, precise and sensitive gas chromatography-mass spectrometry (GC-MS) method coupled with pulse splitless injection technique was developed for the determination of 10 sedative-hypnotics (barbital, amobarbital, phenobarbital, oxazepam, diazepam, nitrazepam, clonazepam, estazolam, alprazolam, triazolam) in human plasma. The drugs spiked in plasma were extracted with ethyl acetate after alkalization with 0.1 mol/L NaOH solution. The organic solvent was evaporated under nitrogen stream, and the residues were redissolved by ethyl acetate. The separation was performed on an HP-5MS column (30 m x 250 microm x 0.25 microm). The analytes were determined and identified using selected ion monitoring (SIM) mode and scan mode, respectively. The internal standard method was used for the determination. The target analytes were well separated from each other on their SIM chromatograms and also on the total ion current (TIC) chromatograms. The blank extract from human plasma gave no peaks that interfered with all the analytes on the chromatogram. The calibration curves for 10 sedative-hypnotics showed excellent linearity. The correlation coefficients of all the drugs were higher than 0.9954. The recoveries of the drugs spiked in human plasma ranged from 92.28% to 111.7%, and the relative standard deviations (RSDs) of intra-day and inter-day determinations were from 4.09% to 14.26%. The detection limits ranged from 2 to 20 microg/L. The method is simple, reliable, rapid and sensitive for the determination and the quantification of 10 sedative-hypnotics in human plasma and seems to be useful in the practice of clinical toxicological cases.

  19. Momentum, heat, and neutral mass transport in convective atmospheric pressure plasma-liquid systems and implications for aqueous targets

    Science.gov (United States)

    Lindsay, Alexander; Anderson, Carly; Slikboer, Elmar; Shannon, Steven; Graves, David

    2015-10-01

    There is a growing interest in the study of plasma-liquid interactions with application to biomedicine, chemical disinfection, agriculture, and other fields. This work models the momentum, heat, and neutral species mass transfer between gas and aqueous phases in the context of a streamer discharge; the qualitative conclusions are generally applicable to plasma-liquid systems. The problem domain is discretized using the finite element method. The most interesting and relevant model result for application purposes is the steep gradients in reactive species at the interface. At the center of where the reactive gas stream impinges on the water surface, the aqueous concentrations of OH and ONOOH decrease by roughly 9 and 4 orders of magnitude respectively within 50 μ m of the interface. Recognizing the limited penetration of reactive plasma species into the aqueous phase is critical to discussions about the therapeutic mechanisms for direct plasma treatment of biological solutions. Other interesting results from this study include the presence of a 10 K temperature drop in the gas boundary layer adjacent to the interface that arises from convective cooling. Though the temperature magnitudes may vary among atmospheric discharge types (different amounts of plasma-gas heating), this relative difference between gas and liquid bulk temperatures is expected to be present for any system in which convection is significant. Accounting for the resulting difference between gas and liquid bulk temperatures has a significant impact on reaction kinetics; factor of two changes in terminal aqueous species concentrations like H2O2, NO2- , and NO3- are observed in this study if the effect of evaporative cooling is not included.

  20. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Young Wook; Nam, Dae Young; Kang, Kyoung Hoon; Ha, Kyung Wook; Han, In Hee; Chang, Byung Kon; Yoon, Mi Kyeong; Lee, Jae Hwi [Chung-Ang University, Seoul (Korea, Republic of)

    2006-02-15

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C{sub 18} column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

  1. Determination of selenium in urine by inductively coupled plasma mass spectrometry: interferences and optimization

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.

    1999-01-01

    and different salts on four selenium isotopes were examined. It was concluded that only Se-82 was usable for quantitative determination in urine as the blank at mass 82 was close to zero. The blank values at masses 76, 77 and 78 varied considerably and differently with different salts and salt concentrations...

  2. Elemental mass spectroscopy of remote surfaces from laser-induced plasmas

    Science.gov (United States)

    Situ, W.; DeYoung, R. J.

    1994-01-01

    The elemental mass analysis of laser-produced ions from Al, Cu, Ge, Ag, and a lunar simulant target when irradiated by a 400-mJ, 8-ns, Nd: YAG laser at 1 x 10(exp 9) W/cm(exp 2), is reported. Ions traveled down a 11.1-m evacuated tube to an ion-trap 1-m time-of-flight (TOF) mass spectrometer where an elemental mass spectrum was recorded. The amount of target material removed per laser pulse and the ionization fraction were measured. The ion spatial distribution was measured at 11.1-m distance and found to be near a fourth-power cosine distribution. These results indicate the ability to mass analyze a surface over a distance of many kilometers for lunar and asteroid surface elemental mass analysis by a remote satellite or lunar rover.

  3. Plasma free metanephrine measurement using automated online solid-phase extraction HPLC tandem mass spectrometry.

    NARCIS (Netherlands)

    Jong, W.H. de; Graham, K.S.; Molen, J.C. van der; Links, T.P.; Morris, M.R.; Ross, H.A.; Vries, E.G.F. de; Kema, I.P.

    2007-01-01

    BACKGROUND: Quantification of plasma free metanephrine (MN) and normetanephrine (NMN) is considered to be the most accurate test for the clinical chemical diagnosis of pheochromocytoma and follow-up of pheochromocytoma patients. Current methods involve laborious, time-consuming, offline sample prepa

  4. Determination of 20 trace elements and arsenic species for a realgar-containing traditional Chinese medicine Niuhuang Jiedu tablets by direct inductively coupled plasma-mass spectrometry and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Jin, Pengfei; Liang, Xiaoli; Xia, Lufeng; Jahouh, Farid; Wang, Rong; Kuang, Yongmei; Hu, Xin

    2016-01-01

    Niuhuang Jiedu tablet (NHJDT) is a realgar-containing traditional Chinese medicine. A direct inductively coupled plasma-mass spectrometry (ICP-MS) method for the simultaneous determination of 20 trace elements (Mg, K, Ca, Na, Fe, As, Zn, Sr, Ba, Cu, Mn, Ni, Pb, V, Cr, Se, Co, Mo, Cd, Hg) in NHJDT, as well as in water, gastric fluid and intestinal fluid was established. Meanwhile, a high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) method was developed for the determination of arsenite (As(III)), arsenate (As(V)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and for the identification of arsenobetaine (AsB) and arsenocholine (AsC) in these extracts. Both methods were fully validated in the respect of linearity, sensitivity, precision, stability and accuracy. The reliability of the ICP-MS method was further evaluated using a certified standard reference material prepared from dried tomato leaves (NIST, SRM 1572a). The analysis showed that some manufacturers formulated lower amount of realgar than required in the Chinese Pharmacopoeia (ChP) in their preparations. In addition, almost same extraction profiles for total As and inorganic As were found in water and in gastrointestinal fluids, while higher extraction rates for other 19 elements were observed in gastrointestinal fluids. Our findings show that the toxicities of Hg, Cu, Cd and Pb in NHJDP are low, while the real As toxicity in NHJDT should be deeply investigated.

  5. Development and Validation of an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Method for Quantitative Analysis of Platinum in Plasma, Urine, and Tissues.

    Science.gov (United States)

    Zhang, Ti; Cai, Shuang; Forrest, Wai Chee; Mohr, Eva; Yang, Qiuhong; Forrest, M Laird

    2016-09-01

    Cisplatin, a platinum chemotherapeutic, is one of the most commonly used chemotherapeutic agents for many solid tumors. In this work, we developed and validated an inductively coupled plasma mass spectrometry (ICP-MS) method for quantitative determination of platinum levels in rat urine, plasma, and tissue matrices including liver, brain, lungs, kidney, muscle, heart, spleen, bladder, and lymph nodes. The tissues were processed using a microwave accelerated reaction system (MARS) system prior to analysis on an Agilent 7500 ICP-MS. According to the Food and Drug Administration guidance for industry, bioanalytical validation parameters of the method, such as selectivity, accuracy, precision, recovery, and stability were evaluated in rat biological samples. Our data suggested that the method was selective for platinum without interferences caused by other presenting elements, and the lower limit of quantification was 0.5 ppb. The accuracy and precision of the method were within 15% variation and the recoveries of platinum for all tissue matrices examined were determined to be 85-115% of the theoretical values. The stability of the platinum-containing solutions, including calibration standards, stock solutions, and processed samples in rat biological matrices was investigated. Results indicated that the samples were stable after three cycles of freeze-thaw and for up to three months. © The Author(s) 2016.

  6. A New Liquid Chromatography-Tandem Mass Spectrometry Method for Determination of Bisoprolol in Human Plasma Samples

    Directory of Open Access Journals (Sweden)

    Gabriela Peste

    2009-01-01

    Full Text Available Liquid chromatography (LC coupled with mass spectrometry (MS detection is one of the most powerful analytical tools for organic compound analysis. The advantages of using LC/MS methods over HPLC methods include: selectivity, chromatographic integrity, peak assignment, structural information, and rapid method development. In this paper, a new liquid chromatography-tandem mass spectrometry (LC-MS/MS method has been developed and validated for the determination of bisoprolol in human plasma samples, using metoprolol as internal standard and liquid-liquid extraction procedure. The assay has proven to be sensitive, specific and reproducible, suitable to determine the bisoprolol concentration, following a single oral administration of a 10 mg bisoprolol tablet in 22 healthy volunteers, in the bioequivalence study of Bisoprolol 10 mg coated tablets, produced by Antibiotice S.A. versus Concor 10 mg, produced by Merck.

  7. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry. Progress report, January 1, 1990--December 31, 1992

    Energy Technology Data Exchange (ETDEWEB)

    Montaser, A.

    1992-09-01

    New high temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. Emphasis was placed on atmospheric pressure He inductively coupled plasmas (ICP) suitable for atomization, excitation, and ionization of elements; simulation and computer modeling of plasma sources with potential for use in spectrochemical analysis; spectroscopic imaging and diagnostic studies of high temperature plasmas, particularly He ICP discharges; and development of new, low-cost sample introduction systems, and examination of techniques for probing the aerosols over a wide range. Refs., 14 figs. (DLC)

  8. On the vanishing electron-mass limit in plasma hydrodynamics in unbounded media

    CERN Document Server

    Donatelli, Donatella; Novotny, Antonin

    2011-01-01

    We consider the zero-electron-mass limit for the Navier-Stokes-Poisson system in unbounded spatial domains. Assuming smallness of the viscosity coefficient and ill-prepared initial data, we show that the asymptotic limit is represented by the incompressible Navier-Stokes system, with a Brinkman damping, in the case when viscosity is proportional to the electron-mass, and by the incompressible Euler system provided the viscosity is dominated by the electron mass. The proof is based on the RAGE theorem and dispersive estimates for acoustic waves, and on the concept of suitable weak solutions for the compressible Navier-Stokes system.

  9. Carotid intima media thickness is associated with plasma lipoprotein-associated phospholipase A(2) mass in nondiabetic subjects but not in patients with type 2 diabetes

    NARCIS (Netherlands)

    Constantinides, Alexander; van Pelt, L. Joost; van Leeuwen, Jeroen J. J.; de Vries, Rindert; Tio, Rene A.; van der Horst, Iwan C. C.; Sluiter, Wim J.; Dullaart, Robin P. F.

    2011-01-01

    Background A recent meta-analysis showed that both plasma lipoprotein-associated phospholipase A(2) (Lp-PLA(2)) mass and activity independently predict cardiovascular events. Notably, Lp-PLA(2) activity but not mass was found to be a determinant of cardiovascular outcome in type 2 diabetes mellitus.

  10. Quantitative Characterization of Gold Nanoparticles by Field-Flow Fractionation Coupled Online with Light Scattering Detection and Inductively Coupled Plasma Mass Spectrometry

    DEFF Research Database (Denmark)

    Schmidt, Bjørn; Löschner, Katrin; Hadrup, Niels

    2011-01-01

    An analytical platform coupling asymmetric flow field-flow fractionation (AF4) with multiangle light scattering (MALS), dynamic light scattering (DLS), and inductively coupled plasma mass spectrometry (ICPMS) was established and used for separation and quantitative determination of size and mass ...

  11. Gas chromatography interfaced with atmospheric pressure ionization-quadrupole time-of-flight-mass spectrometry by low-temperature plasma ionization

    DEFF Research Database (Denmark)

    Norgaard, Asger W.; Kofoed-Sorensen, Vivi; Svensmark, Bo

    2013-01-01

    A low temperature plasma (LTP) ionization interface between a gas chromatograph (GC) and an atmospheric pressure inlet mass spectrometer, was constructed. This enabled time-of-flight mass spectrometric detection of GC-eluting compounds. The performance of the setup was evaluated by injection...

  12. A SIMPLE AND RAPID MATRIX-ASSISTED LASER DESORPTION/IONIZATION TIME OF FLIGHT MASS SPECTROMETRY METHOD TO SCREEN FISH PLASMA SAMPLES FOR ESTROGEN-RESPONSIVE BIOMARKERS

    Science.gov (United States)

    In this study, we describe and evaluate the performance of a simple and rapid mass spectral method for screening fish plasma for estrogen-responsive biomarkers using matrix assisted laster desorption/ionization time of flight mass spectrometry (MALDI-TOF-MS) couopled with a short...

  13. Determination of salvianolic acid C in rat plasma using liquid chromatography-mass spectrometry and its application to pharmacokinetic study.

    Science.gov (United States)

    Song, Junke; Zhang, Wen; Sun, Jialin; Zhang, Xue; Xu, Xiaona; Zhang, Li; Feng, Zhangying; Du, Guanhua

    2016-03-01

    A sensitive and reliable LC-ESI-MS method for the determination of salvianolic acid C in rat plasma has been developed and validated. Plasma samples were prepared by liquid-liquid extraction with ethyl acetate and separated on a Zorbax SB-C18 column (3.5 µm, 2.1 × 100 mm) at a flow rate of 0.3 mL/min using acetonitrile-water as mobile phase. The detection was carried out by a single quadrupole mass spectrometer with electrospray ionization source and selected ion monitoring mode. Linearity was obtained for salvianolic acid C ranging from 5 to 1000 ng/mL. The intra- and inter-day precisions (RSD, %) didn't exceed 9.96%, and the accuracy (RE, %) were all within ±3.64%. The average recoveries of the analyte and internal standard were >89.13%. Salvianolic acid C was proved to be stable during all sample storage, preparation and analytic procedures. The validated method was successfully applied to pharmacokinetic study after oral and intravenous administration of salvianolic acid C to rats. The absolute oral bioavailability of salvianolic acid C was 0.29 ± 0.05%. This method was further applied to simultaneous determination of salvianolic acid A, salvianolic acid B and salvianolic acid C in rat plasma and showed good practicability.

  14. Simultaneous analysis of allopurinol and oxypurinol using a validated liquid chromatography–tandem mass spectrometry method in human plasma

    Directory of Open Access Journals (Sweden)

    Dhiraj M. Rathod

    2017-02-01

    Full Text Available The present study describes a simple, reliable and reproducible liquid chromatography–tandem mass spectrometry method (LC–MS/MS for the simultaneous determination of allopurinol and its active metabolite, oxypurinol in human plasma for a pharmacokinetic/bioequivalence study. After protein precipitation (PPT of 100 µL plasma sample with 1.0% formic acid in acetonitrile, the recovery of the analytes and allopurinol-d2 as an internal standard ranged from 85.36% to 91.20%. The analytes were separated on Hypersil Gold (150 mm×4.6 mm, 5 µm column using 0.1% formic acid-acetonitrile (98:2, v/v as the mobile phase. Quantification was done using electrospray ionization in the positive mode. The calibration concentration range was established from 60.0 to 6000 ng/mL for allopurinol and 80.0–8000 ng/mL for oxypurinol. Matrix effect in human plasma, expressed as IS-normalized matrix factors ranged from 1.003 to 1.030 for both the analytes. The developed method was found suitable for a clinical study with 300 mg allopurinol tablet formulation in healthy subjects.

  15. Multi-element analysis of water decoction of medicine food homology plants using inductively coupled plasma-tandem mass spectrometry

    Science.gov (United States)

    Fu, Liang; Shi, Shu-Yun; Chen, Xiao-Qing

    2017-07-01

    The concentration of twelve trace elements in the water decoction of medicine food homology plants (MFHP) was determined by inductively coupled plasma-tandem mass spectrometry (ICP-MS/MS). Water decoctions of MFHP were analyzed directly using the MS/MS mode after acidification by 1% (v/v) nitric acid. The polyatomic interferences were eliminated by oxygen mass shift, oxygen on-mass, and ammonia mass shift. The accuracy of the method was verified by analysis of standard reference materials. This method was utilized to investigate the water decoction composition of 16 common Chinese MFHPs. The trace elements in the water decoctions of different MFHPs presented significantly different dissolution ratios. The dissolution ratio of V was the lowest (4.21%-14.86%), whereas Zn showed the highest dissolution ratio (24.87%-86.80%). In addition, the dissolution ratio of heavy metallic elements in most MFHP was equal to or was lower than 30%. Therefore, consumption of MHFP decoction could decrease the heavy metal intake associated with MFHP use and reduce the risk of heavy metal poisoning.

  16. A new series of uranium isotope reference materials for investigating the linearity of secondary electron multipliers in isotope mass spectrometry

    Science.gov (United States)

    Richter, S.; Alonso, A.; Aregbe, Y.; Eykens, R.; Kehoe, F.; Kühn, He; Kivel, N.; Verbruggen, A.; Wellum, R.; Taylor, P. D. P.

    2009-04-01

    ) and suitable reference materials for investigating detector linearity are reviewed. Two measurement procedures for applying the IRMM-072 and IRMM-073 (diluted from the remaining fraction of IRMM-072) series as well as the new IRMM-074 series for assessing SEM linearity are suggested. The procedures are tailor-made for the specific instrumental characteristics of thermal ionization mass spectrometers (TIMS) and multiple-collector inductively coupled plasma mass spectrometers (MC-ICPMS) but can be adapted also for further types of isotope ratio mass spectrometers.

  17. Plasma Cell Leukemia Presenting as a Chest Wall Mass: A Case Report

    Directory of Open Access Journals (Sweden)

    Ahmed Ali

    2016-06-01

    Full Text Available Plasma cell leukemia (PCL is an uncommon neoplasm of plasma cells, with an aggressive clinical course and poor outcome, even with current standard of care. It can occur either de novo (primary PCL or as a progression of multiple myeloma (MM. This disease has unique diagnostic criteria but certain genetic markers and clinical features may overlap with MM. Due to the low prevalence of PCL, guidelines on its management are extrapolated from the management of MM and based on small retrospective studies and cases reports/series. We present an interesting case of PCL in a middle-aged African-American male, who was diagnosed incidentally after chest wall imaging for an unrelated complaint. The diagnostic approach, management and outcomes of PCL are discussed.

  18. Plasma Cell Leukemia Presenting as a Chest Wall Mass: A Case Report

    Science.gov (United States)

    Ali, Ahmed; Paul, Yonette; Nwabudike, Stanley Madu; Ogbonna, Onyekachi; Grantham, Mica; Taddesse-Heath, Lekidelu

    2016-01-01

    Plasma cell leukemia (PCL) is an uncommon neoplasm of plasma cells, with an aggressive clinical course and poor outcome, even with current standard of care. It can occur either de novo (primary PCL) or as a progression of multiple myeloma (MM). This disease has unique diagnostic criteria but certain genetic markers and clinical features may overlap with MM. Due to the low prevalence of PCL, guidelines on its management are extrapolated from the management of MM and based on small retrospective studies and cases reports/series. We present an interesting case of PCL in a middle-aged African-American male, who was diagnosed incidentally after chest wall imaging for an unrelated complaint. The diagnostic approach, management and outcomes of PCL are discussed. PMID:27462235

  19. Quantitation of isobaric phosphatidylcholine species in human plasma using a hybrid quadrupole linear ion-trap mass spectrometer.

    Science.gov (United States)

    Zacek, Petr; Bukowski, Michael; Rosenberger, Thad A; Picklo, Matthew

    2016-12-01

    Phosphatidylcholine (PC) species in human plasma are used as biomarkers of disease. PC biomarkers are often limited by the inability to separate isobaric PCs. In this work, we developed a targeted shotgun approach for analysis of isobaric and isomeric PCs. This approach is comprised of two MS methods: a precursor ion scanning (PIS) of mass m/z 184 in positive mode (PIS m/z +184) and MS(3) fragmentation in negative mode, both performed on the same instrument, a hybrid triple quadrupole ion-trap mass spectrometer. The MS(3) experiment identified the FA composition and the relative abundance of isobaric and sn-1, sn-2 positional isomeric PC species, which were subsequently combined with absolute quantitative data obtained by PIS m/z +184 scan. This approach was applied to the analysis of a National Institute of Standards and Technology human blood plasma standard reference material (SRM 1950). We quantified more than 70 PCs and confirmed that a majority are present in isobaric and isomeric mixtures. The FA content determined by this method was comparable to that obtained using GC with flame ionization detection, supporting the quantitative nature of this MS method. This methodology will provide more in-depth biomarker information for clinical and mechanistic studies.

  20. High-sensitivity simultaneous liquid chromatography–tandem mass spectrometry assay of ethinyl estradiol and levonorgestrel in human plasma

    Directory of Open Access Journals (Sweden)

    Abhishek Gandhi

    2015-10-01

    Full Text Available A sensitive and simultaneous liquid chromatography–tandem mass spectrometry method was developed and validated for quantification of ethinyl estradiol and levonorgestrel. The analytes were extracted with methyl-tert-butyl ether: n-hexane (50:50, v/v solvent mixture, followed by dansyl derivatization. The chromatographic separation was performed on a Kinetex C18 (50 mm×4.6 mm, 2.6 µm column with a mobile phase of 0.1% (v/v formic acid in water and acetonitrile in gradient composition. The mass transitions were monitored in electrospray positive ionization mode. The assay exhibited a linear range of 0.100–20.0 ng/mL for levonorgestrel and 4.00–500 pg/mL for ethinyl estradiol in human plasma. A run time of 9.0 min for each sample made it possible to analyze a throughput of more than 100 samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic and bioequivalence studies.

  1. Radionuclide Determination In Surface Water Samples By Inductively Coupled Plasma With Sector Field Mass Spectrometry (ICP-SFMS

    Directory of Open Access Journals (Sweden)

    E. T. Romero-Guzmán

    2016-08-01

    Full Text Available The determination of naturally occurring radionuclides in the environment by inductively coupled plasma mass spectrometry of high resolution (ICP-SFMS has gained recognition over the last fifteen years, relative to the radiometric techniques, as the result of improvement in instrumental performance, sample introduction equipment and sample preparation. With the increase in instrumental sensitivity, it is now possible to measure ultratrace levels of many radioisotopes. The aim of this work was to determined the natural radionuclides (232Th, 234U, 235U and 238U in surface water using Inductively Coupled PlasmaSector Field Mass Spectrometry (ICP-SFMS. The samples were sampling from Lerma river, State of Mexico at february to april 2015. The process of treatment of sample consisted in perform an acid digestion according to the 3015A USEPA method followed of the direct measurement in ICP-SFMS. Results obtained were: a identify the presence of 232Th, 234U, 235U and 238U isotopes in water, b isotopic ratios were for 234U/238U=1.133 ± 0.016. ICPSFMS has gained popularity in the field of radiochemistry, particularly as a method of detection for long lived-actinides.

  2. Determination of Platycodin D and Platycodin D3 in Rat Plasma Using Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Tae-Hyun Kim

    2014-01-01

    Full Text Available Platycodon grandiflorum has long been used as a traditional oriental medicine for respiratory disorder. Platycodin D (PD is known as the main component isolated from the root of PG. A simple and rapid liquid chromatography-tandem mass spectrometry (LC-MS/MS method has been developed and validated for the quantitation of PD in rat plasma. Quantitation was performed on a triple quadrupole mass spectrometer employing electrospray ionization and multiple reaction monitoring in positive ion mode. The total chromatographic run time was 4.0 min, and the calibration curves of PD were linear over the concentration range of 50–10,000 ng/mL in rat plasma. The coefficient of variation and relative error at five QC levels were 1.0 to 8.8% and 0.7 to 8.7%, respectively. After a single oral administration of 500 mg/kg and a single intravenous administration of 25 mg/kg of 3% PD extract (a PG extract including 3% of PD, platycodin D and platycodin D3 were detected and pharmacokinetic parameters were estimated. The oral bioavailability of platycodin D and platycodin D3 was 0.29% and 1.35% in rats at 500 mg/kg of 3% PD extract of PG, respectively. The present method can be applied to pharmacokinetic analysis of platycodins and platycosides of the PG.

  3. Quantitative Mass spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

    Directory of Open Access Journals (Sweden)

    Nahla N. Salama

    2009-01-01

    Full Text Available The present study employs time of flight mass spectrometry for quantitative analysis of the local anesthetic drugs ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL-1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%–102.75% was obtained. The method is accurate (% RE < 5% and reproducible with intra- and inter-assay precision (RSD% < 8.0%. The quantification limit is 23.8 ng mL-1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

  4. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Yanes, Enrique G.; Miller-Ihli, Nancy J.

    2004-06-01

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-μm particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories.

  5. Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yanes, Enrique G. E-mail: yanes@bhnrc.usda.gov; Miller-Ihli, Nancy J. E-mail: miller-ihli@bhnrc.usda.gov

    2004-06-18

    Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-{mu}m particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories.

  6. First identification of dimethoxycinnamic acids in human plasma after coffee intake by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Nagy, Kornél; Redeuil, Karine; Williamson, Gary; Rezzi, Serge; Dionisi, Fabiola; Longet, Karin; Destaillats, Frédéric; Renouf, Mathieu

    2011-01-21

    There is a substantial amount of published literature on the bioavailability of various coffee components including the most abundant metabolites, caffeic and ferulic acids. Surprisingly, to date, the appearance of dimethoxycinnamic acid derivatives in humans has not been reported despite the fact that methylated form of catechol-type polyphenols could help maintain, modify or even improve their biological activities. This study reports an LC-MS method for the detection of dimethoxycinnamic acid in human plasma after treatment with an esterase. Liquid chromatography, including the combination of methanol and acetonitrile as organic eluent, was optimized to resolve all interferences and enable reliable detection and identification of 3,4-dimethoxycinnamic and 3,4-dimethoxy-dihydrocinnamic acids. In addition to the good mass accuracy achieved (better than 5 ppm), tandem mass spectrometric and co-chromatography experiments further confirmed the identity of the compounds. The optimized method was applied to analyze samples obtained immediately, 1 and 10 h after coffee ingestion. The results show that in particular 3,4-dimethoxycinnamic acid appears in high abundance (∼380 nM at 60 min) in plasma upon coffee intake, indicating that it is important to consider these derivatives in future bioavailability and bioefficacy studies.

  7. Rapid Determination of Imatinib in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Jeong Soo; Cho, Eun Gi; Huh, Wooseong; Ko, Jaewook; Jung, Jin Ah; Lee, Sooyoun [Samsung Medical Center, Seoul (Korea, Republic of)

    2013-08-15

    A simple, fast and robust analytical method was developed to determine imatinib in human plasma using liquid chromatography-tandem mass spectrometry with electrospray ionization in the positive ion mode. Imatinib and labeled internal standard were extracted from plasma with a simple protein precipitation. The chromatographic separation was performed using an isocratic elution of mobile phase involving 5.0 mM ammonium formate in water -5.0 mM ammonium formate in methanol (30:70, v/v) over 3.0 min on reversed-stationary phase. The detection was performed using a triple-quadrupole tandem mass spectrometer in multiple-reaction monitoring mode. The developed method was validated with lower limit of quantification of 10 ng/mL. The calibration curve was linear over 10-2000 ng/mL (R{sup 2} > 0.99). The method validation parameters met the acceptance criteria. The spiked samples and standard solutions were stable under conditions for storage and handling. The reliable method was successfully applied to real sample analyses and thus a pharmacokinetic study in 27 healthy Korean male volunteers.

  8. High-sensitivity simultaneous liquid chromatography-tandem mass spectrometry assay of ethinyl estradiol and levonorgestrel in human plasma

    Institute of Scientific and Technical Information of China (English)

    Abhishek Gandhi; Swati Guttikar; Priti Trivedi

    2015-01-01

    A sensitive and simultaneous liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of ethinyl estradiol and levonorgestrel. The analytes were extracted with methyl-tert-butyl ether: n-hexane (50:50, v/v) solvent mixture, followed by dansyl derivatization. The chromatographic separation was performed on a Kinetex C18 (50 mm × 4.6 mm, 2.6μm) column with a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile in gradient composition. The mass transitions were monitored in electrospray positive ionization mode. The assay exhibited a linear range of 0.100-20.0 ng/mL for levonorgestrel and 4.00-500 pg/mL for ethinyl estradiol in human plasma. A run time of 9.0 min for each sample made it possible to analyze a throughput of more than 100 samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic and bioequivalence studies.

  9. Determination of rizatriptan in human plasma by liquid chromatographic-eletrospray tandem mass spectrometry: application to a pharmacokinetic study.

    Science.gov (United States)

    Guo, Ji-fen; Zhang, Ai-jun; Zhao, Ling; Sun, Xiao-hong; Zhao, Yi-min; Gao, Hong-zhi; Liu, Ze-yuan; Qiao, Shan-yi

    2006-01-01

    A sensitive liquid chromatographic-tandem mass spectrometry(LC-MS/MS) method was developed for the determination of rizatriptan in human plasma. The analytes were extracted from plasma samples by liquid-liquid extraction, separated on a Zorbax XDB C8 column (150 x 4.6 mm i.d.) and detected by tandem mass spectrometry with an electrospray ionization interface. Zomitriptan was used as the internal standard. The method had a lower limit of quantitation of 50 pg/mL for rizatriptan, which showed more sensitivity and speed of analysis compared with reported methods. The within- and between-day precision was measured to be below 11.71% and accuracy between -5.87 and 0.86% for all quality control samples. This quantitation method was successfully applied to the evaluation of the pharmacokinetic profiles of rizatriptan after single oral administration of 5, 10 and 15 mg rizatriptan tablets to 10 healthy volunteers (five males and five females).

  10. Liquid chromatography–tandem mass spectrometry method for the estimation of adefovir in human plasma: Application to a pharmacokinetic study

    Directory of Open Access Journals (Sweden)

    Dipanjan Goswami

    2015-06-01

    Full Text Available An analytical method based on solid phase extraction was developed and validated for analysis of adefovir in human plasma. Adefovir-d4 was used as an internal standard and Synergi MAX RP80A (150 mm×4.6 mm, 4 µm column provided the desired chromatographic separation of compounds followed by detection with mass spectrometry. The method used simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode. The calibration curves were linear over the range of 0.50–42.47 ng/mL with the lower limit of quantitation validated at 0.50 ng/mL. Matrix effect was assessed by post-column infusion experiment to monitor phospholipids and post-extraction addition experiment was performed. The degree of matrix effect for adefovir was determined as 7.5% and ion-enhancement in five different lots of human plasma was 7.1% and had no impact on study samples analysis with 4.5 min run time. The intra- and inter-day precision values were within 7.7% and 7.8%, respectively, for adefovir at the lower limit of quantification level. Validated bioanalytical method was successfully applied to clinical sample analysis.

  11. Many flaked particles generated by electric field stress working as an impulsive force in mass-production plasma etching equipment

    Science.gov (United States)

    Kasashima, Yuji; Uesugi, Fumihiko

    2015-09-01

    Particles generated in plasma etching significantly lower production yield. In plasma etching, etching reaction products adhere to the inner chamber walls, gradually forming films, and particles are generated by flaking of the deposited films due to electric field stress that acts boundary between the inner wall and the film. In this study, we have investigated the mechanism of instantaneous generation of many flaked particles using the mass-production reactive ion etching equipment. Particles, which flake off from the films on the ground electrode, are detected by the in-situ particle monitoring system using a sheet-shaped laser beam. The results indicate that the deposited films are severely damaged and flake off as numerous particles when the floating potential at the inner wall suddenly changes. This is because the rapid change in floating potential, observed when unusual wafer movement and micro-arc discharge occur, causes electric field stress working as an impulsive force. The films are easily detached by the impulsive force and many flaked particles are instantaneously generated. This mechanism can occur on not only a ground electrode but a chamber walls, and cause serious contamination in mass-production line. This work was partially supported by JSPS KAKENHI Grant Number B 26870903.

  12. Electrospray-Differential Mobility Hyphenated with Single Particle Inductively Coupled Plasma Mass Spectrometry for Characterization of Nanoparticles and Their Aggregates.

    Science.gov (United States)

    Tan, Jiaojie; Liu, Jingyu; Li, Mingdong; El Hadri, Hind; Hackley, Vincent A; Zachariah, Michael R

    2016-09-01

    The novel hyphenation of electrospray-differential mobility analysis with single particle inductively coupled plasma mass spectrometry (ES-DMA-spICPMS) was demonstrated with the capacity for real-time size, mass, and concentration measurement of nanoparticles (NPs) on a particle-to-particle basis. In this proof-of-concept study, the feasibility of this technique was validated through both concentration and mass calibration using NIST gold NP reference materials. A detection limit of 10(5) NPs mL(-1) was determined under current experimental conditions, which is about 4 orders of magnitude lower in comparison to that of a traditional ES-DMA setup using a condensation particle counter as detector. Furthermore, independent and simultaneous quantification of both size and mass of NPs provides information regarding NP aggregation states. Two demonstrative applications include gold NP mixtures with a broad size range (30-100 nm), and aggregated gold NPs with a primary size of 40 nm. Finally, this technique was shown to be potentially useful for real-world samples with high ionic background due to its ability to remove dissolved ions yielding a cleaner background. Overall, we demonstrate the capacity of this new hyphenated technique for (1) clearly resolving NP populations from a mixture containing a broad size range; (2) accurately measuring a linear relationship, which should inherently exist between mobility size and one-third power of ICPMS mass for spherical NPs; (3) quantifying the early stage propagation of NP aggregation with well-characterized oligomers; and (4) differentiating aggregated NPs and nonaggregated states based on the "apparent density" derived from both DMA size and spICPMS mass.

  13. Determination of sodium cromoglycate in human plasma by liquid chromatography-mass spectrometry in the turbo ion spray mode.

    Science.gov (United States)

    Ozou, M L; Girault, J; Malgouyat, J M; Pasquier, O

    2001-12-25

    A highly sensitivity liquid chromatography-tandem mass spectrometry method has been developed for the quantitation of sodium cromoglycate (SCG) in human plasma. The method was validated over a linear range of 0.100-50.0 ng/ml, using 13C4 sodium cromoglycate as the internal standard. Compounds were extracted from 1.0 ml of lithium heparin plasma by methanol elution of C18 solid-phase extraction cartridges. The dried residue was reconstituted with 100 microl of 0.01 N HCl. and 30 microl was injected onto the LC-MS-MS system. Chromatographic separation was achieved on a C8 (3.5 microm) column with an isocratic mobile phase of methanol-water-0.5 M ammonium acetate (35:64.8:0.2, v/v/v). The analytes were detected with a PE Sciex API 3000 mass spectrometer using turbo ion spray with positive ionization. Ions monitored in the multiple reaction monitoring (MRM) mode were m/z 469.2 (precursor ion) to m/z 245.1 (product ion) for SCG and m/z 473.2 (precursor ion) to m/z 247.1 (product ion) for 13C4 SCG (I.S.). The average recoveries of SCG and the I.S. from human plasma were 91 and 87%, respectively. The low limit of quantitation was 0.100 ng/ml. Results from a 4-day validation study demonstrated excellent precision (C.V.% values were between 1.9 and 6.5%) and accuracy (-5.4 to - 1.2%) across the calibration range of 0.100-50.0 ng/ml.

  14. Determination of trace rare earth elements in gadolinium aluminate by inductively coupled plasma time of flight mass spectrometry

    Science.gov (United States)

    Saha, Abhijit; Deb, S. B.; Nagar, B. K.; Saxena, M. K.

    An analytical methodology was developed for the precise quantification of ten trace rare earth elements (REEs), namely, La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, and Tm, in gadolinium aluminate (GdAlO3) employing an ultrasonic nebulizer (USN)-desolvating device based inductively coupled plasma mass spectrometry (ICP-MS). A microwave digestion procedure was optimized for digesting 100 mg of the refractory oxide using a mixture of sulphuric acid (H2SO4), phosphoric acid (H3PO4) and water (H2O) with 1400 W power, 10 min ramp and 60 min hold time. An USN-desolvating sample introduction system was employed to enhance analyte sensitivities by minimizing their oxide ion formation in the plasma. Studies on the effect of various matrix concentrations on the analyte intensities revealed that precise quantification of the analytes was possible with matrix level of 250 mg L- 1. The possibility of using indium as an internal standard was explored and applied to correct for matrix effect and variation in analyte sensitivity under plasma operating conditions. Individual oxide ion formation yields were determined in matrix matched solution and employed for correcting polyatomic interferences of light REE (LREE) oxide ions on the intensities of middle and heavy rare earth elements (MREEs and HREEs). Recoveries of ≥ 90% were achieved for the analytes employing standard addition technique. Three real samples were analyzed for traces of REEs by the proposed method and cross validated for Eu and Nd by isotope dilution mass spectrometry (IDMS). The results show no significant difference in the values at 95% confidence level. The expanded uncertainty (coverage factor 1σ) in the determination of trace REEs in the samples were found to be between 3 and 8%. The instrument detection limits (IDLs) and the method detection limits (MDLs) for the ten REEs lie in the ranges 1-5 ng L- 1 and 7-64 μg kg- 1 respectively.

  15. Determination of Clarithromycin in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Validation and Application in Clinical Pharmacokinetic Study

    Institute of Scientific and Technical Information of China (English)

    ZHANGXiang-rong; CHENXiao-yan; LIXiao-yan; ZHONGDa-fang

    2004-01-01

    Aim To develop a liquid chromatographic-tandem mass spectrometric (LC-MS-MS) method to determine clarithromycin in human plasma. Methods The analyte and internal standard roxithromycin were extracted from plasma samples by n-nexane-dichloromethane-isopropanel (300:150:15, V/V/V) and chromatographed on a C18 column. The mobile phase consisted of methanol-water-formic acid (80:20:1, V/V/V). Detection was performed on a triple quadrupole tandem mass spectrometer via electrospray ionization source (ESI) in the positive mode. Results The method had a lower limit of quantification of 10.0 ng·mL-1 when 0.2 mL plasma was used. The linear calibration curves were obtained in the concentration range of 10.0-5000 ng·mL-1. The intra-and inter-rum precisions were lower than 3.3% in terms of relative standard deviation (RSD), and the accuracy ranged±0.7% in terms of relative error (RE). Tmax, Cmax, T1/2 and AUC0-24h values were found to be (3.1±2.7)h, (8 750±4 734)ng·mL-1, (5.3±2.2)h, and (5932±2 449)ng·mL-1, respectively, after a single oral dose of 250 mg clarithromycin tablet to 18 volunteers. Conclusion This validated method was successful in the evaluation of pharmacokinetic profiles of clarithromycin tablets administered to 18 healthy male volubteers.

  16. Quantitative comparison of lipoprotein fractions derived from human plasma and serum by liquid chromatography-tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Collins Lisamarie A

    2010-07-01

    Full Text Available Abstract Background Lipoproteins are complex, globular molecules which play essential roles in the transport and metabolism of cholesterol. Their implication in the development of cardiovascular diseases, such as atherosclerosis, has sustained a great deal of interest in these particles. Their various functions, and their contribution to the development of atherosclerosis, are often attributed to their protein constituents, which vary greatly among the different lipoprotein classes. Recent advances in the field of mass spectrometry have provided insight into the array of proteins associated with low-density lipoproteins (LDLs and, even more so, with high-density lipoproteins (HDLs. Plasma and serum are the most commonly used samples for the analysis of lipoproteins. Although these lipoprotein sources are unique, it was our goal to determine whether or not their inherent differences would ultimately affect a quantitative analysis of the LDL and HDL proteomes. To this end, we isolated LDL and HDL fractions with fast protein liquid chromatography-size exclusion chromatography (FPLC-SEC from both human plasma and serum samples from the same individuals. After delipidating these samples, we performed a quantitative proteomic analysis to compare the lipoprotein-associated proteins derived from both plasma and serum. Results Although the primary differences between the samples are found in fibrinogen proteins which are removed from serum, it of interest to note that, with respect to LDL-associated proteins, apolipoproteinB-100 was found at significantly higher levels in serum samples. Complement component 3 was found at significantly higher levels in serum-derived HDL fractions. Both of these proteins are known LDL- and HDL-associated proteins, respectively. Conclusion Overall, the results from our study indicate that both plasma and serum samples are equally suited for proteomic studies, and provide similar results. These findings are particularly

  17. Mass spectrometric signatures of the blood plasma metabolome for disease diagnostics.

    Science.gov (United States)

    Lokhov, Petr G; Balashova, Elena E; Voskresenskaya, Anna A; Trifonova, Oxana P; Maslov, Dmitry L; Archakov, Alexander I

    2016-01-01

    In metabolomics, a large number of small molecules can be detected in a single run. However, metabolomic data do not include the absolute concentrations of each metabolite. Generally, mass spectrometry analyses provide metabolite concentrations that are derived from mass peak intensities, and the peak intensities are strictly dependent on the type of mass spectrometer used, as well as the technical characteristics, options and protocols applied. To convert mass peak intensities to actual concentrations, calibration curves have to be generated for each metabolite, and this represents a significant challenge depending on the number of metabolites that are detected and involved in metabolome-based diagnostics. To overcome this limitation, and to facilitate the development of diagnostic tests based on metabolomics, mass peak intensities may be expressed in quintiles. The present study demonstrates the advantage of this approach. The examples of diagnostic signatures, which were designed in accordance to this approach, are provided for lung and prostate cancer (leading causes of mortality due to cancer in developed countries) and impaired glucose tolerance (which precedes type 2 diabetes, the most common endocrinology disease worldwide).

  18. The relationship of endogenous plasma concentrations of β-Hydroxy β-Methyl Butyrate (HMB) to age and total appendicular lean mass in humans.

    Science.gov (United States)

    Kuriyan, Rebecca; Lokesh, Deepa P; Selvam, Sumithra; Jayakumar, J; Philip, Mamatha G; Shreeram, Sathyavageeswaran; Kurpad, Anura V

    2016-08-01

    The maintenance of muscle mass and muscle strength is important for reducing the risk of chronic diseases. The age- related loss of muscle mass and strength is associated with adverse outcomes of physical disability, frailty and death. β-Hydroxy β-Methyl Butyrate (HMB), a metabolite of leucine, has beneficial effects on muscle mass and strength under various catabolic conditions. The objectives of the present study were to determine if age- related differences existed in endogenous plasma HMB levels, and to assess if HMB levels correlated to total appendicular lean mass and forearm grip strength. Anthropometry, dietary and physical activity assessment, and the estimation of fasting plasma HMB concentrations and handgrip strength were performed on the 305 subjects (children, young adults and older adults). Lean mass, which serves as a surrogate for muscle mass was measured using dual energy X-ray absorptiometry (DEXA). Mean plasma HMB concentrations were significantly lower with increasing age groups, with children having highest mean HMB concentration (plean mass normalized for body weight (%), appendicular lean mass (r=0.37; plean mass and hand grip strength in young adults and older adults group.

  19. Liquid Chromatography-Tandem Mass Spectrometric Assay for Determination of Stavudine in Human Plasma

    Directory of Open Access Journals (Sweden)

    Fengdan Jin

    2014-01-01

    Full Text Available A LC-MS/MS method for determination of stavudine in human plasma was established and validated, and it was applied to the pharmaceutical formulations bioequivalence study. 0.5 mL plasma sample was extracted by liquid-liquid extraction. Stavudine was detected by a LC-MS/MS system. The pharmacokinetic parameters of stavudine in different formulations were calculated by noncompartment model statistics. The method was linear over the concentration ranges 5.00–1000 ng/mL in plasma. The intra- and interassay relative standard deviation (RSD was <10%. The average accuracies for the assay at three concentrations (5.00, 80.0, and 900 ng/mL were from 100.2% to 102.5%. Pharmacokinetic parameters of stavudine reference formulation were obtained as follows: Tmax was 0.6±0.2 h, Cmax was 480.7±150.9 g/L, t1/2 was 1.7±0.4 h, and AUC0-t was 872.8±227.8 g·h/L, and pharmacokinetic parameters of stavudine test formulation were obtained as follows: Tmax was 0.5±0.2 h, Cmax was 537.5±178.5 g/L, t1/2 was 1.7±0.3 h, and AUC0-t was (914.1±284.5 g·h/L. Calculated with AUC0-t, the bioavailability of two formulations was 105.0%.

  20. Fish protein hydrolysate elevates plasma bile acids and reduces visceral adipose tissue mass in rats

    DEFF Research Database (Denmark)

    Liaset, Bjørn; Madsen, Lise; Hao, Qin

    2009-01-01

    Conjugation of bile acids (BAs) to the amino acids taurine or glycine increases their solubility and promotes liver BA secretion. Supplementing diets with taurine or glycine modulates BA metabolism and enhances fecal BA excretion in rats. However, it is still unclear whether dietary proteins...... varying in taurine and glycine contents alter BA metabolism, and thereby modulate the recently discovered systemic effects of BAs. Here we show that rats fed a diet containing saithe fish protein hydrolysate (saithe FPH), rich in taurine and glycine, for 26 days had markedly elevated fasting plasma BA...

  1. Determination of Free Levels of Cinitipride in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Shikha M. N. Roy

    2008-01-01

    4.6 mm, 5 µm i.d.. The assay of cinitapride was linear calibration curve over the range 20.118 pg mL−1 to 2011.797 pg mL−1. Plasma concentrations of cinitapride were determined by LC-MS/MS with a limit of quantification of 20.118 pg mL−1 that allowed an appropriate characterization of the pharmacokinetic profile of cinitapride at the therapeutic dose. The method was successfully applied to the bioequivalence study of cinitapride tablet (1.0 mg administered as a single oral dose.

  2. Determination of folic acid in human plasma using hydrophilic interaction chromatography-tandem mass spectrometry

    NARCIS (Netherlands)

    Garbis, S.D.; Melse-Boonstra, A.; West, C.E.; Breemen, van R.B.

    2001-01-01

    Folic acid is an essential nutrient, and folate deficiency is associated with a variety of disorders including neural tube defects (during pregnancy) and heart disease. A fast, sensitive, and robust HPLC-tandem mass spectrometry (LC-MS-MS) method was developed for the quantification of free folic ac

  3. Determination of folic acid in human plasma using hydrophilic interaction chromatography-tandem mass spectrometry

    NARCIS (Netherlands)

    Garbis, S.D.; Melse-Boonstra, A.; West, C.E.; Breemen, van R.B.

    2001-01-01

    Folic acid is an essential nutrient, and folate deficiency is associated with a variety of disorders including neural tube defects (during pregnancy) and heart disease. A fast, sensitive, and robust HPLC-tandem mass spectrometry (LC-MS-MS) method was developed for the quantification of free folic

  4. Development of a Novel System for Mass Spectrometric Analysis of Cancer-Associated Fucosylation in Plasma α1-Acid Glycoprotein

    Directory of Open Access Journals (Sweden)

    Takayuki Asao

    2013-01-01

    Full Text Available Human plasma α1-acid glycoprotein (AGP from cancer patients and healthy volunteers was purified by sequential application of ion-exchange columns, and N-linked glycans enzymatically released from AGP were labeled and applied to a mass spectrometer. Additionally, a novel software system for use in combination with a mass spectrometer to determine N-linked glycans in AGP was developed. A database with 607 glycans including 453 different glycan structures that were theoretically predicted to be present in AGP was prepared for designing the software called AGPAS. This AGPAS was applied to determine relative abundance of each glycan in the AGP molecules based on mass spectra. It was found that the relative abundance of fucosylated glycans in tri- and tetra-antennary structures (FUCAGP was significantly higher in cancer patients as compared with the healthy group (P<0.001. Furthermore, extremely elevated levels of FUCAGP were found specifically in patients with a poor prognosis but not in patients with a good prognosis. In conclusion, the present software system allowed rapid determination of the primary structures of AGP glycans. The fucosylated glycans as novel tumor markers have clinical relevance in the diagnosis and assessment of cancer progression as well as patient prognosis.

  5. Determination of abacavir, tenofovir, darunavir, and raltegravir in human plasma and saliva using liquid chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Yamada, Eiko; Takagi, Ritsuo; Sudo, Koji; Kato, Shingo

    2015-10-10

    A liquid chromatography-tandem mass spectrometry assay for the determination of abacavir (ABC), tenofovir (TFV), darunavir (DRV), and raltegravir (RAL) in human plasma and saliva was developed and validated to investigate the applicability of saliva as an appropriate specimen for therapeutic drug monitoring. As internal standards, TFV was chosen for ABC, ABC was chosen for TFV, RAL for DRV, and DRV for RAL. Sample preparation involved protein precipitation with acetonitrile, evaporation of solvent using a centrifugal evaporator, and reconstitution by dissolving the residue in mobile phase. Liquid chromatography was performed on a C18 reverse phase column (1.5 × 50 mm, 5 μm) isocratically at a flow rate of 0.2 mL/min using 5mM formic acid-3% (v/v) acetonitrile as the mobile phase for ABC and TFV and 5mM formic acid-35% (v/v) acetonitrile as the mobile phase for DRV and RAL. The run time was 6 min, and the retention time was approximately 2.0 min for TFV, 2.5 min for RAL, and 4-4.5 min for ABC and DRV. Analytes were detected using tandem mass spectrometry in positive electrospray ionization mode. The precursor/product ion transitions (m/z) were 287.3/191.2 for ABC, 288.5/176.2 for TFV, 548.3/392.3 for DRV, and 445.3/109.5 for RAL, and were monitored on a triple-quadrupole mass spectrometer operated in the multiple reaction monitoring mode. The linearity of the assay was assessed in the range 1-10,000 ng/mL for all four drugs. Within-run and between-run mean accuracy, precision, and the extraction recovery for all drugs were -14.5-18.1%, 1.2-13.1%, and 86.0-111.1%, respectively. The proposed assay is sufficiently sensitive and accurate to quantify these drugs in plasma and saliva, and is suitable for investigating the relationship between drug concentrations in plasma and saliva.

  6. The development of an Omegratron plasma ion mass spectrometer for Alcator C-Mod

    Energy Technology Data Exchange (ETDEWEB)

    Thomas, E.E. Jr.

    1993-05-01

    A new diagnostic device, the Omegatron Probe, has been developed to investigate relative impurity levels and impurity charge state distribution in the Alcator C-Mod Tokamak edge plasma. The Omegatron probe consists of two principal components, a ``front-end`` of independently biased grids, arranged in a gridded energy analyzer fashion and a large collection cavity. Particles enter the probe in a thin ``ribbon`` through a knife-edge slit. The grids provide a means to measure and control the parallel energy distribution of the ions. In the collection cavity, an oscillating electric field is applied perpendicularly to the ambient magnetic field. Ions whose cyclotron frequencies are resonant with this electric field oscillation will gain perpendicular energy and be collected. In this way, the probe can be operated in two modes: first, by fixing the potentials on the grids and sweeping frequencies to obtain a `` Z/m spectrum`` of ion species and second, by fixing the frequency and sweeping the grid potentials to obtain the distribution function of an individual impurity species. The Omegatron probe performed successfully in tests on a Hollow Cathode Discharge (HCD) linear plasma column. It obtained measurements of T{sub e} {approx} 5 eV, T{sub i} (H{sup +}) {approx} 2.0 {plus_minus} 0.2 eV, n{sub 0} {approx} 9 {times} 10{sup 15} m{sup {minus}3}, RMS potential fluctuation levels of {approximately} 0.5 {plus_minus} 0.05 {plus_minus} T{sub e}, and obtained ``Z/m`` spectra for the plasma ions (H{sup +}, H{sub 2}{sup +}, He{sup +}). Additional experiments confirmed the theoretical scalings of the f/{delta}f resolution with the applied electric field and magnetic field strengths. The instrument yielded an absolute level of resolution, f/{delta}f, of approximately 2.5 to 3 times the theoretical values. Finally, the results from the HCD are used to project operation on Alcator C-Mod.

  7. STS-46 plasma composition measurements using the EOIM-3 mass spectrometer

    Science.gov (United States)

    Hunton, Donald E.; Trzcinski, Edmund; Gosselin, Roger; Koontz, Steven; Leger, Lubert; Visentine, James T.

    1995-01-01

    One of the active instruments incorporated into the Evaluation of Oxygen Interactions with Materials - 3 experiment was a quadrupole mass spectrometer. The primary objectives for this instrument, which was built by the Air Force Phillips Laboratory and was a veteran of the STS-4 flight in 1982, were to quantify the flux of atomic oxygen striking the test surfaces in the EOIM-3 payload and to detect surface reaction products from the materials in the carousel. Other speakers in this session have covered the results of these experiments. Prior to the 40-hour-long dedicated EOIM-3 mission segment at the end of the STS-46 flight, the authors used the mass spectrometer to make measurements of ion and neutral gas composition in the shuttle environment. About 25 hours of data were collected during a variety of mission events, including Eureca deployment at high altitude and many tethered satellite system operations.

  8. Applications of inductively coupled plasma-mass spectrometry in environmental radiochemistry

    Science.gov (United States)

    Grain, J.S.

    1996-01-01

    The state of the art in ICP-MS is now such that there are few discernible differences between radiochemical and mass spectrometric determinations of longlived radionuclides. Indeed, ICP-MS may provide better (more sensitive) data for many radionuclides, depending upon how one wishes to define "long-lived." In lowlevel determinations, sample preparation remains an important part of the analytical procedure, even with ICP-MS, but the speed and isotopic selectivity of the mass spectrometer appear to offer distinct procedural advantages over radiochemical techniques. Therefore, "radioanalytical" ICP-MS applications should continue to grow, especially in the area of radiation protection, but further research (on efficient sample introduction, for example) and method development may be required to get ICP-MS "off the ground" in the geochemical research areas that have traditionally been supported by radiochemistry.

  9. Lower vs. high momentum mass tomography in Quark-Gluon Plasma

    CERN Document Server

    Djordjevic, Magdalena; Zivkovic, Lidija

    2016-01-01

    We here show that at lower energies single particle suppression for different types of probes exhibit a clear mass hierarchy, which is a direct consequence of the differences in the energy loss, rather than the differences in the initial distributions. On the other hand, we predict that the mass hierarchy is not expected at high energies; i.e. the probes of different masses exhibit nearly the same suppression once high momentum measurements are considered. Moreover, we also argue that the same insensitivity on the probe types is valid for jets as well. In particular, the experimental data in the momentum regions where they exist for both types of probes, show similar suppressions of charged hadrons and inclusive jet data. Finally, the available jet data also show (though with large error bars) an overlap between b-jets (heavy) and inclusive jets (light), which we predict will also be exhibited for soon-to-be-measured charm jets. Consequently, our results suggest that single particles in the momentum region be...

  10. Activation of mass transfer processes at spark plasma sintering of zirconium dioxide

    Science.gov (United States)

    Akarachkin, S. A.; Ivashutenko, A. S.; Martyushev, N. V.

    2016-04-01

    The paper presents the results of numerical simulation of thermal and electric fields' distribution in the graphite moulding tool and in the sintered sample of ZrO2-4%Y2O3 in the course of spark plasma sintering (SPS). The reduction of SPS duration is accounted for the largeness of specific thermal flux towards the sample surface, emitted by the graphite moulding tool. The impact of the electric field on the sample structure leads to emergence of the polarizing processes forcing zirconium ions to shift from lattice sites, which is able to reduce the required value of thermal energy necessary for initiation of a diffusion process. The axial pressure at high temperatures of sintering can lead to plastic deformation of the powder particles.

  11. Multi-elemental analysis of brain tissue from healthy Wistar rats using sector field inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Paul, Mitchell C. [Molecular Structure and Detection Group, School of Environmental and Life Sciences, University of Newcastle, University Drive, Callaghan NSW 2308 (Australia); Parsons, Carl H. [School of Biomedical Science, University of Newcastle, Callaghan NSW 2308 (Australia); Calford, Mike B. [School of Biomedical Science, University of Newcastle, Callaghan NSW 2308 (Australia); Nagy-Felsobuki, Ellak I. von [Molecular Structure and Detection Group, School of Environmental and Life Sciences, University of Newcastle, University Drive, Callaghan NSW 2308 (Australia)]. E-mail: ellak@newcastle.edu.au

    2004-09-20

    The normal distribution of a range of elements in the brain tissue of healthy Wistar rats was established using sector field inductively coupled plasma mass spectrometry. A protocol was developed to determine concentrations of Ag, Cd, Hg, Pb, Bi, U, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As and Se in specific brain regions. The concentrations of these elements were determined in the range of 2{+-}1 (e.g. Cr in diencephalon) to 7558{+-}450 ng ml{sup -1} (e.g. Fe in olfactory bulb). The detection limits of the sixteen elements ranged between 5 and 300 pg ml{sup -1}, with U yielding the lowest and Fe the highest value. The validity of the protocol was assessed by the analysis of SRM 1577B Bovine Liver and brain tissue spike recoveries. A principal component analysis was used to reveal elemental patterns of the brain regions.

  12. Direct Determination of Trace Impurities in High Purity Zinc Oxide by High Resolution Inductively Coupled Plasma Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    XIE Hualin; NIE Xidu; LI Libo; SONG Chuhua

    2006-01-01

    The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) was investigated. To overcome some potentially problematic spectral interference, measurements were acquired in both middle and high resolution modes. The matrix effects due to the presence of excess HCl and zinc were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits ranged from 0.02 μg/g to 6 μg/g depending on the elements.The experimental results for the determination of Na, Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Mo, Cd, Sb and Pb in several high purity zinc oxide powders were presented.

  13. Determination of cadmium, mercury and lead in coal fly ash by slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Liao, H.C.; Jiang, S.J. [National Sun Yat Sen University, Kaohsiung (Taiwan). Dept. of Chemistry

    1999-08-09

    Ultrasonic slurry sampling electrothermal vaporization isotope dilution inductively coupled plasma mass spectrometry (USS-ETV-ID-ICP-MS) was used to the determine Cd, Hg and Pb in coal fly ash samples. Thioacetamide (TAC) was the modifier. Since the sensitivities of the elements studied in coal fly ash slurry and aqueous solution were quite different, isotope dilution method was used for the determination of Cd, Hg and Pb in the coal fly ash samples. The isotope ratios of each element were calculated from the peak areas of each injection peak. This method was applied to the determination of Cd, Hg and Pb in NIST SRM 1633a coal fly ash reference material and a coal fly ash sample collected from Kaohsiung area. Detection limits estimated from standard addition curves were in the range of 24-58, 6-28 and 108-110 ng g{sup -1} for Cd, Hg and Pb, respectively.

  14. Comparison of serum zinc levels measured by inductively coupled plasma mass spectrometry in preschool children with febrile and afebrile seizures.

    Science.gov (United States)

    Lee, Jun-Hwa; Kim, Jeong Hyun

    2012-05-01

    Changes in levels of trace elements have been proposed to underlie febrile seizures. Particularly, low zinc levels have been proposed as related factor of febrile seizure. In this study, we investigated whether mean serum zinc levels differed between children with febrile seizure and afebrile seizure. Using inductively coupled plasma mass spectrometry, serum zinc levels were measured in 288 children who had been diagnosed with febrile seizures (N=248) and afebrile seizures (N=40). Mean serum zinc levels were compared between the 2 groups. Mean serum zinc level was 60.5±12.7 µg/dL in the febrile seizure group and 68.9 ±14.5 µg/dL in the afebrile seizure group. A significant difference in serum zinc levels was observed between the febrile and afebrile seizure groups (Pfebrile seizure were significantly lower than those in children with afebrile seizure.

  15. Aluminium content of some processed foods, raw materials and food additives in China by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Deng, Gui-Fang; Li, Ke; Ma, Jing; Liu, Fen; Dai, Jing-Jing; Li, Hua-Bin

    2011-01-01

    The level of aluminium in 178 processed food samples from Shenzhen city in China was evaluated using inductively coupled plasma-mass spectrometry. Some processed foods contained a concentration of up to 1226 mg/kg, which is about 12 times the Chinese food standard. To establish the main source in these foods, Al levels in the raw materials were determined. However, aluminium concentrations in raw materials were low (0.10-451.5 mg/kg). Therefore, aluminium levels in food additives used in these foods was determined and it was found that some food additives contained a high concentration of aluminium (0.005-57.4 g/kg). The results suggested that, in the interest of public health, food additives containing high concentrations of aluminium should be replaced by those containing less. This study has provided new information on aluminium levels in Chinese processed foods, raw materials and a selection of food additives.

  16. Comparison of ultraviolet femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry analysis in glass, monazite, and zircon.

    Science.gov (United States)

    Poitrasson, Franck; Mao, Xianglei; Mao, Samuel S; Freydier, Rémi; Russo, Richard E

    2003-11-15

    We compared the analytical performance of ultraviolet femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS). The benefit of ultrafast lasers was evaluated regarding thermal-induced chemical fractionation, that is otherwise well known to limit LA-ICPMS. Both lasers had a Gaussian beam energy profile and were tested using the same ablation system and ICPMS analyzer. Resulting crater morphologies and analytical signals showed more straightforward femtosecond laser ablation processes, with minimal thermal effects. Despite a less stable energy output, the ultrafast laser yielded elemental (Pb/U, Pb/Th) and Pb isotopic ratios that were more precise, repeatable, and accurate, even when compared to the best analytical conditions for the nanosecond laser. Measurements on NIST glasses, monazites, and zircon also showed that femtosecond LA-ICPMS calibration was less matrix-matched dependent and therefore more versatile.

  17. Gas and liquid chromatography with inductively coupled plasma mass spectrometry detection for environmental speciation analysis — advances and limitations

    Science.gov (United States)

    Szpunar, Joanna; McSheehy, Shona; Połeć, Kasia; Vacchina, Véronique; Mounicou, Sandra; Rodriguez, Isaac; Łobiński, Ryszard

    2000-07-01

    Recent advances in the coupling of gas chromatography (GC) and high performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP MS) and their role in trace element speciation analysis of environmental materials are presented. The discussion is illustrated with three research examples concerning the following topics: (i) development and coupling of multicapillary microcolumn GC with ICP MS for speciation of organotin in sediment and biological tissue samples; (ii) speciation of arsenic in marine algae by size-exclusion-anion-exchange HPLC-ICP MS; and (iii) speciation of cadmium in plant cell cultures by size-exclusion HPLC-ICP MS. Particular attention is paid to the problem of signal identification in ICP MS chromatograms; the potential of electrospray MS/MS for this purpose is highlighted.

  18. Determination of trace mercury species by high performance liquid chromatography-inductively coupled plasma mass spectrometry after cloud point extraction.

    Science.gov (United States)

    Chen, Haiting; Chen, Jianguo; Jin, Xianzhong; Wei, Danyi

    2009-12-30

    A sensitive method for speciation analysis of inorganic mercury (Hg(2+)) and methyl mercury (MeHg(+)) has been developed by using high performance liquid chromatography (HPLC) combined with inductively coupled plasma mass spectrometry (ICP-MS) after cloud point extraction. The analytes were complexed with sodium diethyldithiocarbamate (DDTC) and preconcentrated by a non-ionic surfactant Triton X-114. Mercury species were effectively separated by HPLC in less than 6 min. The enhancement factors for 25 mL sample solution were 42 and 21, and the limits of detection were 4 and 10 ng L(-1) for Hg(2+) and MeHg(+), respectively. The developed method was successfully applied to the determination of trace amount of mercury species in environmental and biological samples.

  19. Intelligent Analysis of Samples by Semiquantitative Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) Technique: A Review.

    Science.gov (United States)

    Krzciuk, Karina

    2016-07-03

    Inductively coupled plasma-mass spectrometry (ICP-MS) is a popular and routine analytical method that has been used for determination of trace elements since the 1980s. It provides fast quantitative analysis and allows the determination of more than 70 elements with good accuracy and very low detection limits, but requires an intricate calibration procedure. In analyses of samples for which very low detection limits are not required a semiquantitative ICP-MS analysis mode can be used. This approach is more time- and cost-effective, and it uses a simple calibration procedure. This article presents a critical review of the semiquantitative (SQ) mode of ICP-MS and describes current and future applications of SQ analysis.

  20. The determination of low level trace elements in coals by laser ablation-inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Booth, C.A.; Spears, D.A.; Krause, P.; Cox, A.G. [University of Sheffield, Sheffield (United Kingdom). Dept. of Earth Sciences

    1999-11-01

    The rapid determination of elements present in low level concentrations in bituminous coals is possible using laser abalation-inductively coupled plasma-mass spectrometry (l.a.-i.c.p.-m.s.). A wide range of trace elements can routinely be determined using this technique but it is for environmentally sensitive elements, such as As, Cd, Mo, Sb, Se and Hg, that it is of most use due to the low levels of detection. Calibration of the i.c.p.-m.s. was achieved using a series of uncertified coals and the method evaluated using the South African certified coals, Sarm 18, 19 and 20. A critical evaluation of the data obtained shows that for many of the elements studied the results obtained are both accurate and precise, even at very low concentrations, with the limits of detection for all of the elements being in the {mu}g/kg (parts per billion) range. 6 refs., 3 figs., 9 tabs.

  1. Novel applications of high performance ion chromatography-inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    CERN Document Server

    Hann, S

    2001-01-01

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) the components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates.

  2. Use of dried blood spots and inductively coupled plasma mass spectrometry for multi-element determination in blood.

    Science.gov (United States)

    Vacchina, Véronique; Huin, Vincent; Hulo, Sébastien; Cuny, Damien; Broly, Franck; Renom, Gilles; Perini, Jean-Marc

    2014-07-01

    The paper describes the development of an inductively coupled plasma mass spectrometry (ICP MS) method for multitrace element determination in dried blood spots (DBSs). The analytical conditions were optimized using Seronorm™ L-3 and L-1 Certified Reference Materials. The best results were obtained by sampling blood drops on a decontaminated PVDF filter membrane. After drying under metal-free conditions, the DBSs underwent acidic digestion and were analyzed with ICP MS. The method was then validated for As, Cd, Cu, Pb, Mo, Se and Zn. Using a matrix-matched calibration curve, the recovery levels ranged from 96% to 117%. The repeatability and reproducibility were generally below 15%. Limits of quantification ranging from 0.5 to 50 μg/L. In order to investigate the analytical procedure under real sampling conditions, the results obtained from DBSs and liquid blood aliquots (less subject to contamination) from two adult subjects were compared.

  3. Rapid and Sensitive Liquid Chromatography-Tandem Mass Spectrometry for Quantification of Glycyrrhctic Acid in Human Plasma

    Institute of Scientific and Technical Information of China (English)

    TIAN Li; GAO Xiao-li; CHEN Xiao-yan; ZHONG Da-fang; ZHANG Yi-fan; DAI Xiao-jian

    2011-01-01

    A simple, rapid and sensitive liquid chromatography-tandem mass spectrometry(LC-MS/MS) for the determination of glycyrrhetic acid in human plasma with ginsenoside Rh2 as internal standard was developed and validated. The plasma samples were prepared via liquid-liquid extraction with ethyl acetate. Chromatographic separation was accomplished on a Venusil MP-C1s(50 mm×2.1 mm, 5 μm i.d.) column at 25 ℃. The mobile phase consisted of acetonitrile/5 mmol·L-1 ammonium acetate(10:90, volume ratio) at a flow rate of 0.4 mL/min. Negative electrospray ionization was utilized as the ionization source. Glycyrrhetic acid and internal standard were determined via the mutiple reaction monitoring of precursor→production ion transitions at m/z 469→425, 409 and m/z 621→ 161,respectively. Each sample was chromatographed within 2.5 min. The lower limit of quantification was 0.50 ng/mL for 200 μL of plasma sample and the linear range was from 0.50 ng/mL to 800 ng/mL. The intra- and inter-day precisions were less than 8.76% in terms of relative standard deviation(RSD), and the accuracy was within a range of -3.25% -1.32% in terms of relative error(RE). The method was successfully applied to the pharmacokinetic studies of glycyrrhetic acid in healthy male Chinese volunteers after a single oral administration of 75 mg of glycyrrhizin.

  4. Quantification of neomangiferin in rat plasma by liquid chromatography–tandem mass spectrometry and its application to bioavailability study

    Directory of Open Access Journals (Sweden)

    Bo Yang

    2016-10-01

    Full Text Available Neomangiferin, a natural C-glucosyl xanthone, has recently received a great deal of attention due to its multiple biological activities. In this study, a rapid and sensitive ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS method for the quantification of neomangiferin in rat plasma was developed. Using chloramphenicol as an internal standard (IS, plasma samples were subjected to a direct protein precipitation process using methanol (containing 0.05% formic acid. Quantification was performed by multiple reactions monitoring (MRM method, with the transitions of the parent ions to the product ions of m/z 583.1→330.9 for NG and m/z 321.1→151.9 for IS. The assay was shown to be linear over the range of 0.2–400 ng/mL, with a lower limit of quantification of 0.2 ng/mL. Mean recovery of neomangiferin in plasma was in the range of 97.76%–101.94%. Relative standard deviations (RSDs of intra-day and inter-day precision were both <10%. The accuracy of the method ranged from 94.20% to 108.72%. This method was successfully applied to pharmacokinetic study of neomangiferin after intravenous (2 mg/kg and intragastric (10 mg/kg administration for the first time. The oral absolute bioavailability of neomangiferin was estimated to be 0.53%±0.08% with an elimination half-life (t1/2 value of 2.74±0.92 h, indicating its poor absorption and/or strong metabolism in vivo.

  5. Methods of gas purification and effect on the ion composition in an RF atmospheric pressure plasma jet investigated by mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grosse-Kreul, Simon; Huebner, Simon; Schneider, Simon; Keudell, Achim von; Benedikt, Jan [Ruhr-Universitaet Bochum, Institute for Experimental Physics II, Bochum (Germany)

    2016-12-15

    The analysis of the ion chemistry of atmospheric pressure plasmas is essential to evaluate ionic reaction pathways during plasma-surface or plasma-analyte interactions. In this contribution, the ion chemistry of a radio-frequency atmospheric pressure plasma jet (μ-APPJ) operated in helium is investigated by mass spectrometry (MS). It is found, that the ion composition is extremely sensitive to impurities such as N{sub 2}, O{sub 2} and H{sub 2}O. Without gas purification, protonated water cluster ions of the form H{sup +}(H{sub 2}O){sub n} are dominating downstream the positive ion mass spectrum. However, even after careful feed gas purification to the sub-ppm level using a molecular sieve trap and a liquid nitrogen trap as well as operation of the plasma in a controlled atmosphere, the positive ion mass spectrum is strongly influenced by residual trace gases. The observations support the idea that species with a low ionization energy serve as a major source of electrons in atmospheric pressure helium plasmas. Similarly, the neutral density of atomic nitrogen measured by MS in a He/N{sub 2} mixture is varying up to a factor 3, demonstrating the significant influence of impurities on the neutral species chemistry as well. (orig.)

  6. Simultaneous quantification of caffeine and its three primary metabolites in rat plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Choi, Eu Jin; Bae, Soo Hyeon; Park, Jung Bae; Kwon, Min Jo; Jang, Su Min; Zheng, Yu Fen; Lee, Young Sun; Lee, Su-Jun; Bae, Soo Kyung

    2013-12-01

    A rapid, sensitive, simple and accurate LC-MS/MS method for the simultaneous quantitation of caffeine, and its three primary metabolites, theobromine, paraxanthine, and theophylline, in rat plasma was developed and validated. Chromatographic separation was performed on an Agilent Poroshell 120 EC-C18 column using 1 μg/mL acetaminophen as an internal standard. Each sample was run at 0.5 mL/min for a total run time of 7 min/sample. Detection and quantification were performed using a mass spectrometer in selected reaction-monitoring mode with positive electrospray ionization. The lower limit of quantification was 5 ng/mL for all analytes with linear ranges up to 5000 ng/mL for caffeine and 1000 ng/mL for its metabolites. The coefficient of variation for assay precision was less than 12.6%, with an accuracy of 93.5-114%. The assay was successfully applied to determine plasma concentrations of caffeine, theobromine, paraxanthine, and theophylline in rat administered various energy drinks containing the same caffeine content. Various energy drinks exhibited considerable variability in the pharmacokinetic profiles of caffeine and its three primary metabolites, even containing the same caffeine. Different additives of energy drinks might contribute to these results. Copyright © 2013 Elsevier Ltd. All rights reserved.

  7. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    2016-01-01

    Levetiracetam (LEV) is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS) for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size) without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time), the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient's plasma sample using less than 550 μL of organic solvent. PMID:27830105

  8. Determination of lanthanides in rock samples by inductively coupled plasma mass spectrometry using thorium as oxide and hydroxide correction standard

    Science.gov (United States)

    Raut, Narendra M.; Huang, Li-Shing; Aggarwal, Suresh K.; Lin, King-Chuen

    2003-05-01

    Determination of lanthanides by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) using modified mathematical correction method has been studied. Normally, the ICP-MS analysis of middle and heavier lanthanides becomes difficult by severe spectroscopic overlap of M +, MO + or MOH + ions from lighter lanthanides and Ba. A correction method based on a single element oxide yield measurement, is a simple approach to correct for the above spectroscopic overlaps. But the uncertainty in the oxide and hydroxide yields measurement of lanthanides and barium over a long period of time can lead to inaccurate results even under fixed plasma conditions. To correct this, thorium was adopted as an oxide and hydroxide correction standard. Using a ratio of lanthanide oxide yield to thorium oxide yield, the lanthanide correction factors (LCF) were established and incorporated in the mathematical correction scheme. The same factors were also established for hydroxide correction. The proposed modified correction scheme was applied to the determination of lanthanides by ICP-MS from the USGS Standard Rock samples AGV-1 and G-2. The results are in good agreement with the reported values. The method also proved to be useful in isotopic ratio measurement of lanthanides having severe isobaric overlaps.

  9. Simultaneous determination of buprenorphine, norbuprenorphine and naloxone in human plasma by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Liu, Yongzhen; Li, Xiaohua; Xu, Allan; Nasser, Azmi F; Heidbreder, Christian

    2016-02-20

    A simple, sensitive and rapid liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) method was developed and validated for simultaneous quantification of naloxone, buprenorphine and its metabolite norbuprenorphine in human plasma. Human plasma samples were extracted using a single step liquid-liquid extraction, and then separated on an Imtakt Unison UK-C18 column (2.1×50mm, 3μm) using alkaline mobile phases with gradient elution. All of the analytes were detected in positive ion mode using multiple reaction monitoring (MRM). The method was validated and the specificity, linearity, lower limit of quantitation, precision, accuracy, recoveries and stability were determined. The linear range was 20-10000pg/mL for buprenorphine and norbuprenorphine; and 1-500pg/mL for naloxone. The correlation coefficient (R(2)) values for all three analytes were ≥0.995. The precision and accuracy for intra-day and inter-day were 63% and matrix effects were tracked by the deuterated internal standards (IS) with the IS-normalized matrix factor ranging from 0.96 to 1.33 for all three analytes. The validated method was successfully applied in a clinical pharmacokinetic study with low dose administration of sublingual buprenorphine and naloxone.

  10. Ultra-performance liquid chromatography-tandem mass spectrometry method for the analysis of amphetamines in plasma.

    Science.gov (United States)

    Fernández, María del Mar Ramírez; Samyn, Nele

    2011-10-01

    A fast and selective ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS) method for the determination of amphetamines (amphetamine, methamphetamine, methylenedioxymethamphetamine, methylenedioxyamphetamine, methylenedioxyethylamphetamine, ephedrine, and p-methoxyamphetamine) in plasma has been developed and validated. Sample preparation was performed by liquid-liquid extraction using ethyl acetate. For optimized chromatographic performance with repeatable retention times, narrow and symmetrical peaks, and focusing all analytes at the column inlet, a gradient start, with acid mobile phase consisting of 0.1% formic acid and methanol was chosen. Positive electrospray ionization MS-MS detection was performed with two multiple reaction monitoring transitions for each analyte. Deuteriumlabeled internal standards were used for five of the analytes. The limit of detection was in the range 0.25-1.25 ng/mL, and the limit of quantification was fixed at the lowest calibrator of 2.5 ng/mL for all of the compounds. The RSD values of the intra- and interassay precision and accuracy were lower than 11% at four concentration levels, including two external quality controls. No or only minor matrix effects were observed, and the extraction method presented recoveries higher than 93% for all the compounds. Total run time, including equilibration, was 12 min. The method is routinely used at the National Institute of Criminalistics and Criminology for quantitative determination of the main amphetamines in plasma from forensic and driving under the influence cases.

  11. The quick and ultrasensitive determination of K in NaI using inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Arnquist, Isaac J.; Hoppe, Eric W.

    2017-04-01

    A highly sensitive, novel and quick assay method utilizing inductively coupled plasma mass spectrometry was developed for the determination of K in NaI powders and NaI(Tl) scintillator crystals for use in ultralow background applications. The determination of K (viz. 40K), as well as Th and U and their daughters, is important in ultralow background detector materials to ensure incorporation of materials of sufficiently high radiopurity. Through the use of improved instrumentation, cool plasma operating conditions, and meticulously clean sample preparations, detection limits of 11 fg natK∙g-1 (or 341 pBq 40K∙kg-1) was attained for K in pure water. Detection limits in the sample matrix (i.e., NaI) were 0.529 ng natK∙g NaI-1 (or 16.4 Bq 40K∙kg NaI -1). A number of different precursor NaI powder samples and NaI(Tl) scintillator crystals were assayed for their K content. Determinations ranged from 0.757 – 31.4 ng natK∙g NaI-1. This method allows for the screening of materials to unprecedented levels in a fraction of the time compared to gamma counting techniques, providing a useful method for a more effective screening tool of K in ultralow background detector materials.

  12. Plasma and Magnetic Field Characteristics of Solar Coronal Mass Ejections in Relation to Geomagnetic Storm Intensity and Variability

    CERN Document Server

    Liu, Ying D; Wang, Rui; Yang, Zhongwei; Zhu, Bei; Liu, Yi A; Luhmann, Janet G; Richardson, John D

    2015-01-01

    The largest geomagnetic storms of solar cycle 24 so far occurred on 2015 March 17 and June 22 with $D_{\\rm st}$ minima of $-223$ and $-195$ nT, respectively. Both of the geomagnetic storms show a multi-step development. We examine the plasma and magnetic field characteristics of the driving coronal mass ejections (CMEs) in connection with the development of the geomagnetic storms. A particular effort is to reconstruct the in situ structure using a Grad-Shafranov technique and compare the reconstruction results with solar observations, which gives a larger spatial perspective of the source conditions than one-dimensional in situ measurements. Key results are obtained concerning how the plasma and magnetic field characteristics of CMEs control the geomagnetic storm intensity and variability: (1) a sheath-ejecta-ejecta mechanism and a sheath-sheath-ejecta scenario are proposed for the multi-step development of the 2015 March 17 and June 22 geomagnetic storms, respectively; (2) two contrasting cases of how the CM...

  13. A Quantitative Analysis of Memantine in Human Plasma Using Ultra Performance Liquid Chromatography/Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Sunil K. Dubey

    2009-01-01

    Full Text Available The aim of this study is to compare the single-dose oral bioavailability of memantine hydrochloride 10 mg tablets of Ranbaxy Laboratories Limited, with NAMENDA™ tablets (containing memantine hydrochloride 10 mg of Forest Pharmaceuticals Inc. in healthy, adult, human subjects under fasting condition. The study was carried out as 2-way crossover design on 8 subjects in fasting and fed conditions. The plasma samples were obtained over a 72 h post dose in each period. Plasma memantine samples were analyzed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS with positive ion electro spray ionization using multiple reactions monitoring (MRM. A sensitive, reproducible, accurate and validated LC-MS/MS method with limit of quantification (LOQ 0.200 ng/mL was used to analyze memantine. Ln transformed AUC0-72 and Cmax were assessed for bioequivalence using 90% confidence interval (CI. 90% confidence intervals for the ratio of test and reference (Ratio of least-squares mean for ln-transformed AUC0-72 and Cmax were within the regulatory acceptance criteria of 80-125%.

  14. Simultaneous determination of irbesartan and hydrochlorothiazide in human plasma using HPLC coupled with tandem mass spectrometry: Application to bioequivalence studies.

    Science.gov (United States)

    Tutunji, Lara F; Tutunji, Maha F; Alzoubi, Mamoun I; Khabbas, Manal H; Arida, Adi I

    2010-03-11

    A sensitive, specific and selective liquid chromatography/tandem mass spectrometric method has been developed and validated for the simultaneous determination of irbesartan and hydrochlorothiazide in human plasma. Plasma samples were prepared using protein precipitation with acetonitrile, the two analytes and the internal standard losartan were separated on a reverse phase C(18) column (50mmx4mm, 3microm) using water with 2.5% formic acid, methanol and acetonitrile (40:45:15, v/v/v (%)) as a mobile phase (flow rate of 0.70mL/min). Irbesartan and hydrochlorothiazide were ionized using ESI source in negative ion mode, prior to detection by multiple reaction monitoring (MRM) mode while monitoring at the following transitions: m/z 296-->269 and m/z 296-->205 for hydrochlorothiazide, 427-->175 for irbesartan. Linearity was demonstrated over the concentration range 0.06-6.00microg/mL for irbesartan and 1.00-112.00ng/mL for hydrochlorothiazide. The developed and validated method was successfully applied to a bioequivalence study of irbesartan (300mg) with hydrochlorothiazide (12.5mg) tablet in healthy volunteers (N=36).

  15. Determination of roxatidine in human plasma by liquid chromatography/electrospray mass spectrometry and application to a clinical pharmacokinetic study.

    Science.gov (United States)

    Shin, Beom Soo; Choi, Jin Won; Balthasar, Joseph P; Hong, Deok Ki; Kim, Jung Jun; Yoo, Sun Dong

    2007-01-01

    A rapid and sensitive liquid chromatography/mass spectrometry (LC/MS) method was developed and validated for the determination of roxatidine in human plasma. Roxatidine was extracted by single liquid-liquid extraction with tert-butyl methyl ether, and the chromatographic separation was performed on a C8 column. The total analytical run time was relatively short (5 min), and the limit of assay quantification was 2 ng/mL using 0.1 mL of human plasma. Roxatidine and the internal standard, propranolol, were monitored in selected ion monitoring (SIM) mode at m/z 307.3 and 260.3, respectively. The standard curve was linear over a concentration range from 2-500 ng/mL, and the correlation coefficients were >0.999. The mean intra- and inter-day assay accuracy ranged from 103.4-108.8% and 102.3-110.0%, respectively, and the mean intra- and inter-day precision was between 3.3-8.8% and 5.3-6.2%, respectively. The developed assay method was successfully applied to a pharmacokinetic study in human volunteers after oral administration of roxatidine acetate hydrochloride at a dose of 75 mg.

  16. Quantification of roxatidine in human plasma by liquid chromatography electrospray ionization tandem mass spectrometry: application to a bioequivalence study.

    Science.gov (United States)

    Ryu, Ju-Hee; Choi, Sang-Jun; Lee, Heon-Woo; Choi, Seung-Ki; Lee, Kyung-Tae

    2008-12-01

    A sensitive and specific method using a one-step liquid-liquid extraction (LLE) with ethyl acetate followed by high-performance liquid chromatography (HPLC) coupled with positive ion electrospray ionization tandem mass spectrometry (ESI-MS/MS) detection was developed and validated for the determination of roxatidine in human plasma using famotidine as an internal standard (IS). Data acquisition was carried out in multiple reaction monitoring (MRM) mode, by monitoring the transitions m/z 307.3-->107.1 for roxatidine and m/z 338.4-->189.1 for famotidine. Chromatographic separation was performed on a reverse phase Hydrosphere C(18) column at 0.2 mL min(-1) using a mixture of methanol-ammonium formate buffer as mobile phase (20:80, v/v; adjusted to pH 3.9 with formic acid). The achieved lower limit of quantification (LLOQ) was 1.0 ng mL(-1) and the standard calibration curve for roxatidine was linear (r(2)=0.998) over the studied range (1-1000 ng mL(-1)) with acceptable accuracy and precision. Roxatidine was found to be stable in human plasma samples under short-, long-term storage and processing conditions. The developed method was validated and successfully applied to the bioequivalence study of roxatidine administrated as a single oral dose (75 mg as roxatidine acetate hydrochloride) to healthy female Korean volunteers.

  17. Determination of Levetiracetam in Human Plasma by Dispersive Liquid-Liquid Microextraction Followed by Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Greyce Kelly Steinhorst Alcantara

    2016-01-01

    Full Text Available Levetiracetam (LEV is an antiepileptic drug that is clinically effective in generalized and partial epilepsy syndromes. The use of this drug has been increasing in clinical practice and intra- or -interindividual variability has been exhibited for special population. For this reason, bioanalytical methods are required for drug monitoring in biological matrices. So this work presents a dispersive liquid-liquid microextraction method followed by gas chromatography-mass spectrometry (DLLME-GC-MS for LEV quantification in human plasma. However, due to the matrix complexity a previous purification step is required. Unlike other pretreatment techniques presented in the literature, for the first time, a procedure employing ultrafiltration tubes Amicon® (10 kDa porous size without organic solvent consumption was developed. GC-MS analyses were carried out using a linear temperature program, capillary fused silica column, and helium as the carrier gas. DLLME optimized parameters were type and volume of extraction and dispersing solvents, salt addition, and vortex agitation time. Under chosen parameters (extraction solvent: chloroform, 130 μL; dispersing solvent: isopropyl alcohol, 400 μL; no salt addition and no vortex agitation time, the method was completely validated and all parameters were in agreement with the literature recommendations. LEV was quantified in patient’s plasma sample using less than 550 μL of organic solvent.

  18. Determination of L-ephedrine, pseudoephedrine, and caffeine in rat plasma by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Cooper, Stephen D; Fletcher, Brenda L; Silinski, Melanie A Rehder; Brown, Sherri S; Lodge, Jon W; Fernando, Reshan A; Collins, Bradley J

    2011-07-01

    A rapid and simple liquid chromatography tandem mass spectrometry method was developed and validated for the simultaneous determination of L-ephedrine, pseudoephedrine, and caffeine in male Fisher-344 rat plasma at nanogram-per-milliliter concentrations for use in support of toxicology studies. Only 25 μL of plasma is required, and extraction is performed using a simple, single-step protein precipitation. The method was validated over a range of 2.09 to 5460 ng/mL for L-ephedrine, 2.09 to 5050 ng/mL for pseudoephedrine and 2.03 to 5340 ng/mL for caffeine. A binary gradient elution at 0.3 mL/min was used with a Waters XBridge Phenyl (2.1 × 150 mm, 3.5 μm) column and a Waters XBridge Phenyl 2.1- × 10-mm guard column at ambient temperature. The mobile phase consisted of 10 mM ammonium acetate in water (pH 5.0) and methanol. Caffeine trimethyl-(13)C(3) was used as the internal standard. The method was evaluated for linearity, recovery, precision, accuracy, and stability, and it was successfully applied in toxicokinetic studies of ephedrine, administered alone, in combination with caffeine, and in the herbal source Ma Huang.

  19. Simultaneous quantitation of acetylsalicylic acid and clopidogrel along with their metabolites in human plasma using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Chhonker, Yashpal S; Pandey, Chandra P; Chandasana, Hardik; Laxman, Tulsankar Sachin; Prasad, Yarra Durga; Narain, V S; Dikshit, Madhu; Bhatta, Rabi S

    2016-03-01

    The interest in therapeutic drug monitoring has increased over the last few years. Inter- and intra-patient variability in pharmacokinetics, plasma concentration related toxicity and success of therapy have stressed the need of frequent therapeutic drug monitoring of the drugs. A sensitive, selective and rapid liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method was developed for the simultaneous quantification of acetylsalicylic acid (aspirin), salicylic acid, clopidogrel and carboxylic acid metabolite of clopidogrel in human plasma. The chromatographic separations were achieved on Waters Symmetry Shield(TM) C18 column (150 × 4.6 mm, 5 µm) using 3.5 mm ammonium acetate (pH 3.5)-acetonitrile (10:90, v/v) as mobile phase at a flow rate of 0.75 mL/min. The present method was successfully applied for therapeutic drug monitoring of aspirin and clopidogrel in 67 patients with coronary artery disease.

  20. Thallium Analysis in Environmental Samples by Inductively Coupled Plasma Mass Spectrometry; Analisis de Talio en Muestras Ambientales por Espectrometria de Masas con Fuente de Plasma de Acoplamiento Inductivo

    Energy Technology Data Exchange (ETDEWEB)

    Higueras, I.; Fernandez, M.; Conde, E.; Gajate, A.

    2008-08-06

    Due to its high toxicity, thallium has been considered by the US Environmental Protection Agency as one of the priority pollutants to be controlled. While being a highly toxic element, thallium has been studied to a much lesser degree than other toxic elements, mainly because thallium is often undetected by classical analytical methods. Thallium is a rare and dispersed element that occurs mainly in sulfur-containing ores. Thus, it is a potential pollutant to surrounding environment, if Tl-rich mineral and/or their industrial wastes are not properly disposed. In this work an Inductively Coupled Plasma Mass Spectrometry analytical procedure has been developed in order to determine thallium in environmental solid samples and its application to the study of this element as a potential pollutant associated with natural and anthropogenic activities. The analytical procedure has been validated by the use of appropriate reference materials, and through the isotope dilution technique as a primary method of measurement. Finally, the developed procedure has been applied to several samples from a mining area, as one of the scenarios where thallium it is likely to occur. (Author) 87 refs.

  1. Ultra-sensitive quantification of lysozyme based on element chelate labeling and capillary electrophoresis–inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yang, MingWei [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, Fujian Provincial Key Lab of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350108, Fujian (China); Department of Chemistry, Florida International University, Miami, FL 33199 (United States); Wu, WeiHua; Ruan, YaJuan; Huang, LiMei [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, Fujian Provincial Key Lab of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350108, Fujian (China); Wu, Zujian [Department of Plant Protection, Fujian Agriculture and Forest University, Fuzhou 350002, Fujian (China); Cai, Yong [Department of Chemistry, Florida International University, Miami, FL 33199 (United States); Fu, FengFu, E-mail: fengfu@fzu.edu.cn [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, Fujian Provincial Key Lab of Analysis and Detection for Food Safety, Department of Chemistry, Fuzhou University, Fuzhou 350108, Fujian (China); Department of Plant Protection, Fujian Agriculture and Forest University, Fuzhou 350002, Fujian (China)

    2014-02-17

    Graphical abstract: An ultra-sensitive method for the determination of lysozyme was developed based on the Gd{sup 3+} chelate labeling and CE–ICP–MS. The proposed method has an extremely low detection limit of 3.89 attomole and has been successfully used to detect lysozyme in saliva sample, showing excellent reliability. The success of the present method provides a new possibility for biological assays and clinical diagnoses. -- Highlights: •An ultra-sensitive method for detecting lysozyme based on CE–ICP–MS was described. •The proposed method has an extremely low detection limit of 3.89 attomole. •It can be used to detect trace lysozyme in saliva sample with a satisfied recovery. •The method provides a new potential for sensitive detection of low-abundant proteins. -- Abstract: In this study, an ultra-sensitive method for the quantification of lysozyme based on the Gd{sup 3+} diethylenetriamine-N,N,N′,N″,N″-pentaacetic acid labeling and capillary electrophoresis–inductively coupled plasma mass spectrometry (CE–ICP–MS) was described. The Gd{sup 3+}-tagged lysozyme was effectively separated by capillary electrophoresis (CE) and sensitively determined by inductively coupled plasma mass spectrometry (ICP–MS). Based on the gadolinium-tagging and CE–ICP–MS, the lysozyme was determined within 12 min with an extremely low detection limit of 3.89 attomole (3.89 × 10{sup −11} mol L{sup −1} for 100 nL of sample injection) and a RSD < 6% (n = 5). The proposed method has been successfully used to detect lysozyme in saliva samples with a recovery of 91–106%, suggesting that our method is sensitive and reliable. The success of the present method provides a new potential for the biological assays and sensitive detection of low-abundant proteins.

  2. Validated ultra-performance liquid chromatography tandem mass spectrometry method for the determination of pramipexole in human plasma.

    Science.gov (United States)

    Yadav, Manish; Rao, Rajasekhar; Kurani, Hemal; Rathod, Jaysukh; Patel, Rakesh; Singhal, Puran; Shrivastav, Pranav S

    2010-11-01

    A sensitive and high throughput ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) method has been developed for the determination of pramipexole, a dopamine agonist, in human plasma. Sample preparation involved liquid-liquid extraction of pramipexole and ranitidine as the internal standard (IS) in ethyl acetate from 100 μL human plasma. The chromatographic separation is achieved on a Waters Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) analytical column using an isocratic mobile phase, consisting of 10 mM ammonium formate (pH 7.50)-acetonitrile (15:85, v/v), at a flow-rate of 0.5 mL/min. The precursor → product ion transition for pramipexole (m/z 212.1 → 153.0) and IS (m/z 315.0 → 176.1) were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring (MRM) and positive ion mode. The method was validated over a wide dynamic concentration range of 20-4020 pg/mL. Matrix effect is assessed by post-column infusion experiment and the process efficiency were 91.9% and 85.7% for pramipexole and IS, respectively. The method is rugged and rapid with a total run time of 1.5 min and is applied to a bioequivalence study of 0.25 mg PPX tablet formulation in 30 healthy Indian male subjects under fasting condition.

  3. Determination of ginsenoside compound K in human plasma by liquid chromatography–tandem mass spectrometry of lithium adducts

    Science.gov (United States)

    Chen, Yunhui; Lu, Youming; Yang, Yong; Chen, Xiaoyan; Zhu, Liang; Zhong, Dafang

    2015-01-01

    Ginsenoside compound K (GCK), the main metabolite of protopanaxadiol constituents of Panax ginseng, easily produces alkali metal adduct ions during mass spectrometry particularly with lithium. Accordingly, we have developed a rapid and sensitive liquid chromatography–tandem mass spectrometric method for analysis of GCK in human plasma based on formation of a lithium adduct. The analyte and paclitaxel (internal standard) were extracted from 50 µL human plasma using methyl tert-butyl ether. Chromatographic separation was performed on a Phenomenex Gemini C18 column (50 mm×2.0 mm; 5 μm) using stepwise gradient elution with acetonitrile–water and 0.2 mmol/L lithium carbonate at a flow rate of 0.5 mL/min. Detection was performed in the positive ion mode using multiple reaction monitoring of the transitions at m/z 629→449 for the GCK-lithium adduct and m/z 860→292 for the adduct of paclitaxel. The assay was linear in the concentration range 1.00–1000 ng/mL (r2>0.9988) with intra- and inter-day precision of ±8.4% and accuracy in the range of −4.8% to 6.5%. Recovery, stability and matrix effects were all satisfactory. The method was successfully applied to a pharmacokinetic study involving administration of a single GCK 50 mg tablet to healthy Chinese volunteers. PMID:26579476

  4. Evaluation of number concentration quantification by single-particle inductively coupled plasma mass spectrometry: microsecond vs. millisecond dwell times.

    Science.gov (United States)

    Abad-Álvaro, Isabel; Peña-Vázquez, Elena; Bolea, Eduardo; Bermejo-Barrera, Pilar; Castillo, Juan R; Laborda, Francisco

    2016-07-01

    The quality of the quantitative information in single-particle inductively coupled plasma mass spectrometry (SP-ICP-MS) depends directly on the number concentration of the nanoparticles in the sample analyzed, which is proportional to the flux of nanoparticles through the plasma. Particle number concentrations must be selected in accordance with the data acquisition frequency, to control the precision from counting statistics and the bias, which is produced by the occurrence of multiple-particle events recorded as single-particle events. With quadrupole mass spectrometers, the frequency of data acquisition is directly controlled by the dwell time. The effect of dwell times from milli- to microseconds (10 ms, 5 ms, 100 μs, and 50 μs) on the quality of the quantitative data has been studied. Working with dwell times in the millisecond range, precision figures about 5 % were achieved, whereas using microsecond dwell times, the suitable fluxes of nanoparticles are higher and precision was reduced down to 1 %; this was independent of the dwell time selected. Moreover, due to the lower occurrence of multiple-nanoparticle events, linear ranges are wider when dwell times equal to or shorter than 100 μs are used. A calculation tool is provided to determine the optimal concentration for any instrument or experimental conditions selected. On the other hand, the use of dwell times in the microsecond range reduces significantly the contribution of the background and/or the presence of dissolved species, in comparison with the use of millisecond dwell times. Although the use of dwell times equal to or shorter than 100 μs offers improved performance working in single-particle mode, the use of conventional dwell times (3-10 ms) should not be discarded, once their limitations are known.

  5. Laser ablation-inductively coupled plasma mass spectrometry: an emerging technology for detecting rare cells in tissue sections.

    Science.gov (United States)

    Managh, Amy J; Hutchinson, Robert W; Riquelme, Paloma; Broichhausen, Christiane; Wege, Anja K; Ritter, Uwe; Ahrens, Norbert; Koehl, Gudrun E; Walter, Lisa; Florian, Christian; Schlitt, Hans J; Reid, Helen J; Geissler, Edward K; Sharp, Barry L; Hutchinson, James A

    2014-09-01

    Administering immunoregulatory cells to patients as medicinal agents is a potentially revolutionary approach to the treatment of immunologically mediated diseases. Presently, there are no satisfactory, clinically applicable methods of tracking human cells in patients with adequate spatial resolution and target cell specificity over a sufficient period of time. Laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) represents a potential solution to the problem of detecting very rare cells in tissues. In this article, this exquisitely sensitive technique is applied to the tracking of gold-labeled human regulatory macrophages (Mregs) in immunodeficient mice. Optimal conditions for labeling Mregs with 50-nm gold particles were investigated by exposing Mregs in culture to variable concentrations of label: Mregs incubated with 3.5 × 10(9) particles/ml for 1 h incorporated an average of 3.39 × 10(8) Au atoms/cell without loss of cell viability. Analysis of single, gold-labeled Mregs by LA-ICP-MS registered an average of 1.9 × 10(5) counts/cell. Under these conditions, 100% labeling efficiency was achieved, and label was retained by Mregs for ≥36 h. Gold-labeled Mregs adhered to glass surfaces; after 24 h of culture, it was possible to colabel these cells with human-specific (154)Sm-tagged anti-HLA-DR or (174)Yb-tagged anti-CD45 mAbs. Following injection into immunodeficient mice, signals from gold-labeled human Mregs could be detected in mouse lung, liver, and spleen for at least 7 d by solution-based inductively coupled plasma mass spectrometry and LA-ICP-MS. These promising results indicate that LA-ICP-MS tissue imaging has great potential as an analytical technique in immunology. Copyright © 2014 by The American Association of Immunologists, Inc.

  6. Speciation of Selenium in Selenium-Enriched Sunflower Oil by High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry/Electrospray-Orbitrap Tandem Mass Spectrometry.

    Science.gov (United States)

    Bierla, Katarzyna; Flis-Borsuk, Anna; Suchocki, Piotr; Szpunar, Joanna; Lobinski, Ryszard

    2016-06-22

    The reaction of sunflower oil with selenite produces a complex mixture of selenitriglycerides with antioxidant and anticancer properties. To obtain insight into the identity and characteristics of the species formed, an analytical approach based on the combination of high-performance liquid chromatography (HPLC) with (78)Se-specific selenium detection by inductively coupled plasma mass spectrometry (ICP MS) and high-resolution (100 000), high mass accuracy (sunflower oil dissolved in isopropanol and methanol extract of the oil containing 65% selenium. HPLC-ICP MS showed 14 peaks, 11 of which could also be detected in the methanol extract. Isotopic patterns corresponding to molecules with one or two selenium atoms could be attributed by Orbitrap MS at the retention times corresponding to the HPLC-ICP MS peak apexes. Structural data for these species were acquired by MS(2) and MS(3) fragmentation of protonated or sodiated ions using high-energy collisional dissociation (HCD). A total of 11 selenium-containing triglycerol derivatives resulting from the oxidation of one or two double bonds of linoleic acid and analogous derivatives of glycerol-mixed linoleate(s)/oleinate(s) have been identified for the first time. The presence of these species was confirmed by the targeted analysis in the total oil isopropanol solution. Their identification corroborated the predicted elution order in reversed-phase chromatography: LLL (glycerol trilinoleate), LLO (glycerol dilinoleate-oleinate), LOO (glycerol linoleate-dioleinate), OOO (glycerol trioleinate), of which the extrapolation allowed for the prediction of the identity [glycerol dioleinate-stearate (OOS) and glycerol oleinate-distearate (OSS)] of the nonpolar species detected by ICP MS in the oil but not detected by electrospray MS.

  7.   Plant Phosphoproteomics: Analysis of Plasma Membrane Transporters by Mass Spectrometry

    DEFF Research Database (Denmark)

    Ye, Juanying; Rudashevskaya, Elena; Young, Clifford

    phosphorylation. Due to the low abundance of phosphoprotein, the specific enrichment prior to MS analysis is necessary. Plant proton pump (H+-ATPase) is an enzyme controls the major transport processes in the plant, such as root nutrient uptake. Moreover, this pump has been proposed to be involved in other......  Phosphorylation is a key regulatory factor in all aspects of eukaryotic biology including the regulation of plant membrane-bound transport proteins. To date, mass spectrometry (MS) has been introduced as powerful technology for study of post translational modifications (PTMs), including protein...

  8. Determination of Metformin in Human Plasma by Liquid Chromatography-tandem Mass Spectrometric Assay

    Institute of Scientific and Technical Information of China (English)

    WANG Jian; WANG Ying-wu; GU Jing-kai; WU Yi; WANG Yan

    2005-01-01

    @@ Introduction Metformin (1,1-dimethylbiguanide) (Fig. 1) is an oral anti-hyperglycemic agent used in the treatment of non-insulin-dependent diabetes mellitus (type Ⅱ). Owing to its weight-decreasing and serum lipid-normalizing effects, it is especially recommended for obese patients[1,2] Various analytical methods have been described for the measurement of metformin in biological fluids, including gas chromatography(GC)[3-5], capillary electrophoresis (CE)[6] and HPLC[7~16]with UV detection[7-12,17] HPLC-Mass spectrometry (LC/APCIMS/MS ) offers an attractive alternative to HPLC[18].

  9. A high-throughput method for liquid chromatography-tandem mass spectrometry determination of plasma alkylresorcinols, biomarkers of whole grain wheat and rye intake

    DEFF Research Database (Denmark)

    Ross, Alastair B; Svelander, Cecilia; Savolainen, Otto I;

    2016-01-01

    supported extraction methods for extracting alkylresorcinols from plasma and improved a normal-phase liquid chromatography coupled to a tandem mass spectrometer method to reduce sample analysis time. The method was validated and compared with gas chromatography-mass spectrometry analysis. Sample preparation...... with HybridSPE supported extraction was most effective for alkylresorcinol extraction, with recoveries of 77-82% from 100 μl of plasma. The use of 96-well plates allowed extraction of 160 samples per day. Using a 5-cm NH2 column and heptane reduced run times to 3 min. The new method had a limit of detection...

  10. Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives

    DEFF Research Database (Denmark)

    Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente

    2006-01-01

    Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material, t...... analysis of bromine-containing preservatives in commercially available cosmetic products.......Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material...

  11. Analysis of bioethanol samples through Inductively Coupled Plasma Mass Spectrometry with a total sample consumption system

    Science.gov (United States)

    Sánchez, Carlos; Lienemann, Charles-Philippe; Todolí, Jose-Luis

    2016-10-01

    Bioethanol real samples have been directly analyzed through ICP-MS by means of the so called High Temperature Torch Integrated Sample Introduction System (hTISIS). Because bioethanol samples may contain water, experiments have been carried out in order to determine the effect of ethanol concentration on the ICP-MS response. The ethanol content studied went from 0 to 50%, because higher alcohol concentrations led to carbon deposits on the ICP-MS interface. The spectrometer default spray chamber (double pass) equipped with a glass concentric pneumatic micronebulizer has been taken as the reference system. Two flow regimes have been evaluated: continuous sample aspiration at 25 μL min- 1 and 5 μL air-segmented sample injection. hTISIS temperature has been shown to be critical, in fact ICP-MS sensitivity increased with this variable up to 100-200 °C depending on the solution tested. Higher chamber temperatures led to either a drop in signal or a plateau. Compared with the reference system, the hTISIS improved the sensitivities by a factor included within the 4 to 8 range while average detection limits were 6 times lower for the latter device. Regarding the influence of the ethanol concentration on sensitivity, it has been observed that an increase in the temperature was not enough to eliminate the interferences. It was also necessary to modify the torch position with respect to the ICP-MS interface to overcome them. This fact was likely due to the different extent of ion plasma radial diffusion encountered as a function of the matrix when working at high chamber temperatures. When the torch was moved 1 mm plasma down axis, ethanolic and aqueous solutions provided statistically equal sensitivities. A preconcentration procedure has been applied in order to validate the methodology. It has been found that, under optimum conditions from the point of view of matrix effects, recoveries for spiked samples were close to 100%. Furthermore, analytical concentrations for real

  12. Determination of trace rare earth elements in gadolinium aluminate by inductively coupled plasma time of flight mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Saha, Abhijit; Deb, S.B.; Nagar, B.K.; Saxena, M.K., E-mail: saxenamk@barc.gov.in

    2014-04-01

    An analytical methodology was developed for the precise quantification of ten trace rare earth elements (REEs), namely, La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, and Tm, in gadolinium aluminate (GdAlO{sub 3}) employing an ultrasonic nebulizer (USN)-desolvating device based inductively coupled plasma mass spectrometry (ICP-MS). A microwave digestion procedure was optimized for digesting 100 mg of the refractory oxide using a mixture of sulphuric acid (H{sub 2}SO{sub 4}), phosphoric acid (H{sub 3}PO{sub 4}) and water (H{sub 2}O) with 1400 W power, 10 min ramp and 60 min hold time. An USN-desolvating sample introduction system was employed to enhance analyte sensitivities by minimizing their oxide ion formation in the plasma. Studies on the effect of various matrix concentrations on the analyte intensities revealed that precise quantification of the analytes was possible with matrix level of 250 mg L{sup −1}. The possibility of using indium as an internal standard was explored and applied to correct for matrix effect and variation in analyte sensitivity under plasma operating conditions. Individual oxide ion formation yields were determined in matrix matched solution and employed for correcting polyatomic interferences of light REE (LREE) oxide ions on the intensities of middle and heavy rare earth elements (MREEs and HREEs). Recoveries of ≥ 90% were achieved for the analytes employing standard addition technique. Three real samples were analyzed for traces of REEs by the proposed method and cross validated for Eu and Nd by isotope dilution mass spectrometry (IDMS). The results show no significant difference in the values at 95% confidence level. The expanded uncertainty (coverage factor 1σ) in the determination of trace REEs in the samples were found to be between 3 and 8%. The instrument detection limits (IDLs) and the method detection limits (MDLs) for the ten REEs lie in the ranges 1–5 ng L{sup −1} and 7–64 μg kg{sup −1} respectively. - Highlights: • A

  13. Rapid and simultaneous quantification of levetiracetam and its carboxylic metabolite in human plasma by liquid chromatography tandem mass spectrometry.

    Directory of Open Access Journals (Sweden)

    Li-Ling Yeap

    Full Text Available A simple liquid chromatography tandem mass spectrometry method was developed and validated according to the guidelines of the US Food and Drug Administration and the European Medicines Agency for a simultaneous quantification of levetiracetam (LEV and its metabolite, UCB L057 in the plasma of patients. A 0.050 mL plasma sample was prepared by a simple and direct protein precipitation with 0.450 mL acetonitrile (ACN containing 1 µg/mL of internal standard (IS, diphenhydramine, then vortex mixed and centrifuged. A 0.100 mL of the clear supernatant was diluted with 0.400 mL water and well mixed. A 0.010 mL of the resultant solution was injected into an Agilent Zorbax SB-C18 (2.1 mm×100 mm, 3.5 µm column with an isocratic elution at 0.5 mL/min using a mixture of 0.1% formic acid in water and ACN (40:60 v/v. Detection was performed using an AB Sciex API 3000 triple quadrupole mass spectrometer, equipped with a Turbo Ion Spray source, operating in a positive mode: LEV at transition 171.1>154.1, UCB L057 at 172.5>126.1, and IS at 256.3>167.3; with an assay run time of 2 minutes. The lower limit of quantification (LLOQ for both LEV and UCB L057 was validated at 0.5 µg/mL, while their lower limit of detection (LOD was 0.25 µg/mL. The calibration curves were linear between 0.5 and 100 µg/mL for both analytes. The inaccuracy and imprecision of both intra-assay and inter-assay were less than 10%. Matrix effects were consistent between sources of plasma and the recoveries of all compounds were between 100% and 110%. Stability was established under various storage and processing conditions. The carryovers from both LEV and UCB L057 were less than 6% of the LLOQ and 0.13% of the IS. This assay method has been successfully applied to a population pharmacokinetic study of LEV in patients with epilepsy.

  14. Rapid and simultaneous quantification of levetiracetam and its carboxylic metabolite in human plasma by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Yeap, Li-Ling; Lo, Yoke-Lin

    2014-01-01

    A simple liquid chromatography tandem mass spectrometry method was developed and validated according to the guidelines of the US Food and Drug Administration and the European Medicines Agency for a simultaneous quantification of levetiracetam (LEV) and its metabolite, UCB L057 in the plasma of patients. A 0.050 mL plasma sample was prepared by a simple and direct protein precipitation with 0.450 mL acetonitrile (ACN) containing 1 µg/mL of internal standard (IS, diphenhydramine), then vortex mixed and centrifuged. A 0.100 mL of the clear supernatant was diluted with 0.400 mL water and well mixed. A 0.010 mL of the resultant solution was injected into an Agilent Zorbax SB-C18 (2.1 mm×100 mm, 3.5 µm) column with an isocratic elution at 0.5 mL/min using a mixture of 0.1% formic acid in water and ACN (40:60 v/v). Detection was performed using an AB Sciex API 3000 triple quadrupole mass spectrometer, equipped with a Turbo Ion Spray source, operating in a positive mode: LEV at transition 171.1>154.1, UCB L057 at 172.5>126.1, and IS at 256.3>167.3; with an assay run time of 2 minutes. The lower limit of quantification (LLOQ) for both LEV and UCB L057 was validated at 0.5 µg/mL, while their lower limit of detection (LOD) was 0.25 µg/mL. The calibration curves were linear between 0.5 and 100 µg/mL for both analytes. The inaccuracy and imprecision of both intra-assay and inter-assay were less than 10%. Matrix effects were consistent between sources of plasma and the recoveries of all compounds were between 100% and 110%. Stability was established under various storage and processing conditions. The carryovers from both LEV and UCB L057 were less than 6% of the LLOQ and 0.13% of the IS. This assay method has been successfully applied to a population pharmacokinetic study of LEV in patients with epilepsy.

  15. Comparison of unit resolution SRM and TOF-MS at 12,000 mass resolution for quantitative bioanalysis of 11 steroids from human plasma.

    Science.gov (United States)

    Rousu, Timo; Tolonen, Ari

    2012-03-01

    The use of high-resolution MS systems for quantitative bioanalysis is a growing field, even though a clear majority of bioanalytical methods are still based on MS/MS with triple quadrupole (QqQ) instrumentation. The recent advances in TOF-MS technology have provided increased linear range and a high selectivity of detection by increased mass resolution and mass accuracy, making these instruments attractive for quantitative analysis due to lack of a need for compound-specific detection reaction optimization and their capability to collect data for a high number of compounds by sensitive wide mass range data acquisition. Here, 11 steroids spiked to human plasma were analyzed by LC-MS using both a QqQ MS system and a TOF instrument operating at 12,000 mass resolution. Sample preparation was performed by hybrid SPE technology. The LOD were 0.5-5 and 0.5-20 ng/ml in plasma for all analytes with QqQ and TOF-MS detection, respectively. Although the results show wider linear range and slightly better sensitivity for most of the compounds with QqQ in comparison to TOF, acceptable performance was obtained for most of the compounds within the range of LOD to 2000 ng/ml (in plasma), this was also the case with LC-TOF-MS analysis. The main problem in TOF-MS analysis at 12,000 mass resolution from plasma was selectivity rather than sensitivity or linear range.

  16. Energetics and Propagation of Coronal Mass Ejections in Different Plasma Environments

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Based on previous work, we investigate the propagation of CMEs in amore realistic plasma environment than the isothermal atmosphere, and find thatMach number MA for the inflow into the reconnection site has to be at least 0.013in order to give a plausible eruption (compared to MA = 0.005 for the isothermalatmosphere). Taking MA = 0.1, we find that the energy output and the electricfield induced inside the current sheet match the temporal behavior inferred fromthe energetic, long duration, CME-associated X-ray events. The results indicatethat catastrophic loss of equilibrium in the coronal magnetic field provides the mostpromising mechanism for major solar eruptions, and that the more energetic theeruption is, the earlier the associated flare peaks. The variation of the output powerwith the background field strength revealed by our calculations implies the poor cor-relation between slow CMEs and solar flares. This work also further confirms theexplanation we proposed for the peculiar motion of giant X-ray arches and anoma-lous post-flare loops. Their kinematic pattern and observed heights are determined by the local Alfven speed and its variation with height.

  17. Rapid and simple extraction of lipids from blood plasma and urine for liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Bang, Dae Young; Byeon, Seul Kee; Moon, Myeong Hee

    2014-02-28

    A simple and fast lipid extraction method from human blood plasma and urine is introduced in this study. The effective lipid extraction from biological systems with a minimization of the matrix effect is important for the successful qualitative and quantitative analysis of lipids in liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). The method described here is based on the modification of the quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction method, which was originally developed for pesticide residue analysis in food, for the purpose of isolating lipids from biological fluids. Applicability of QuEChERS method for lipids was evaluated by varying organic solvents for the extraction/partitioning of lipids in MgSO4/CH3COONa for the removal of water and by varying sorbents (primary secondary amines, graphitized carbon black, silica, strong anion exchange resins and C18 particles) for the dispersive solid-phase extraction (dSPE) step. This study shows that 2:1 (v/v) CHCl3/CH3OH is effective in the extraction/partitioning step and that 50mg of C18 particles (for 0.1mL plasma and 1mL of urine) are more suitable for sample cleanup for the dSPE step of the QuEChERS method. Matrix effects were calculated by comparing the recovery values of lipid standards spiked to both plasma and urine samples after extraction with those of the same standards in a neat solution using nanoflow LC-ESI-MS/MS, resulting in improved MS signals due to the decrease of the ion suppression compared to the conventional Folch method. The modified QuEChERS method was applied to lipid extracts from both human urine and plasma samples, demonstrating that it can be powerfully utilized for high-speed (lipids compared to the Folch method, with equivalent or slightly improved results in lipid identification using nLC-ESI-MS/MS.

  18. Plasma pharmacokinetics and bioavailability of verticillin A following different routes of administration in mice using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Wang, Jiang; Zhu, Xiaohua; Kolli, Shamala; Wang, Hongyan; Pearce, Cedric J; Oberlies, Nicholas H; Phelps, Mitch A

    2017-05-30

    Verticillin A is a natural product isolated from fungal cultures and has displayed potent antibiotic, antiviral, nematocidal, and anticancer properties in vitro. While in vivo studies have been limited due to sparse supply, the in vivo efficacy data that does exist demonstrates potent anti-tumor activity in murine cancer models. The current study aims to investigate the pharmacokinetics and bioavailability of verticillin A in mice to provide guidance for further efficacy assessment in mouse models. A sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for the quantification of verticillin A in mouse plasma. Sample preparation was accomplished through protein precipitation, and chromatographic separation was achieved on an Agilent Zorbax Extend C18 column with a security guard cartridge C8 using a binary gradient with mobile phase A (water/0.1% formic acid) and B (ACN/0.1% formic acid) at a flow rate of 400μl/min. Elution of verticillin A and internal standard, hesperetin, occurred at 4.87 and 2.06min, respectively. The total chromatographic run time was 8min, and the assay was linear in the concentration range of 1-1000nM. The within- and between day precisions and accuracy were in the range of 2.58-8.71 and 90-105%, respectively. The assay was applied to determine plasma drug concentration in a mouse pharmacokinetic study. It was found that intraperitoneal dosing of 3mg/kg resulted in high systemic exposure and achieved Cmax of 110nM with plasma concentrations sustained above 10nM for the 24-h duration of the study. Intravenous and oral dosing achieved observed Cmax of 73nM and 9nM, respectively. Oral dosing resulted in an approximate 9% bioavailability. Comparing with previously published in vitro studies that demonstrated verticillin A is active in the 20nM to 130nM range, the pharmacokinetic data demonstrate similar levels are achieved in mouse plasma via intravenous or intraperitoneal dosing routes

  19. Rapid analysis of pharmaceuticals and personal care products in fish plasma micro-aliquots using liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Chen, Fangfang; Gong, Zhiyuan; Kelly, Barry C

    2015-02-27

    A sensitive analytical method based on liquid-liquid extraction (LLE) and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed for rapid analysis of 11 pharmaceuticals and personal care products (PPCPs) in fish plasma micro-aliquots (∼20μL). Target PPCPs included, bisphenol A, carbamazepine, diclofenac, fluoxetine, gemfibrozil, ibuprofen, naproxen, risperidone, sertraline, simvastatin and triclosan. A relatively quicker and cheaper LLE procedure exhibited comparable analyte recoveries with solid-phase extraction. Rapid separation and analysis of target compounds in fish plasma extracts was achieved by employing a high efficiency C-18 HPLC column (Agilent Poroshell 120 SB-C18, 2.1mm×50mm, 2.7μm) and fast polarity switching, enabling effective monitoring of positive and negative ions in a single 9min run. With the exception of bisphenol A, which exhibited relatively high background contamination, method detection limits of individual PPCPs ranged between 0.15 and 0.69pg/μL, while method quantification limits were between 0.05 and 2.3pg/μL. Mean matrix effect (ME) values ranged between 65 and 156% for the various target analytes. Isotope dilution quantification using isotopically labelled internal surrogates was utilized to correct for signal suppression or enhancement and analyte losses during sample preparation. The method was evaluated by analysis of 20μL plasma micro-aliquots collected from zebrafish (Danio rerio) from a laboratory bioaccumulation study, which included control group fish (no exposure), as well as fish exposed to environmentally relevant concentrations of PPCPs. Using the developed LC-MS/MS based method, concentrations of the studied PPCPs were consistently detected in the low pg/μL (ppb) range. The method may be useful for investigations requiring fast, reliable concentration measurements of PPCPs in fish plasma. In particular, the method may be applicable for in situ contaminant biomonitoring, as well as

  20. RAPID DETERMINATION OF 237 NP AND PU ISOTOPES IN WATER BY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.; Jones, V.; Culligan, B.; Nichols, S.; Noyes, G.

    2010-06-23

    A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of {sup 237}Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry; a hybrid approach. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry so that long and short-lived Pu isotopes can be measured successfully. The method allows for simultaneous extraction of 20 samples (including QC samples) in 4 to 6 hours, and can also be used for emergency response. {sup 239}Pu, {sup 242}Pu and {sup 237}Np were measured by ICP-MS, while {sup 236}Pu, {sup 238}Pu, and {sup 239}Pu were measured by alpha spectrometry.

  1. DETERMINATION OF 237NP AND PU ISOTOPES IN LARGE SOIL SAMPLES BY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.

    2010-07-26

    A new method for the determination of {sup 237}Np and Pu isotopes in large soil samples has been developed that provides enhanced uranium removal to facilitate assay by inductively coupled plasma mass spectrometry (ICP-MS). This method allows rapid preconcentration and separation of plutonium and neptunium in large soil samples for the measurement of {sup 237}Np and Pu isotopes by ICP-MS. {sup 238}U can interfere with {sup 239}Pu measurement by ICP-MS as {sup 238}UH{sup +} mass overlap and {sup 237}Np via {sup 238}U peak tailing. The method provides enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then transferring Pu to DGA resin for additional purification. The decontamination factor for removal of uranium from plutonium for this method is greater than 1 x 10{sup 6}. Alpha spectrometry can also be applied so that the shorter-lived {sup 238}Pu isotope can be measured successfully. {sup 239}Pu, {sup 242}Pu and {sup 237}Np were measured by ICP-MS, while {sup 236}Pu and {sup 238}Pu were measured by alpha spectrometry.

  2. Direct and Sensitive Detection of CWA Simulants by Active Capillary Plasma Ionization Coupled to a Handheld Ion Trap Mass Spectrometer

    Science.gov (United States)

    Wolf, Jan-Christoph; Etter, Raphael; Schaer, Martin; Siegenthaler, Peter; Zenobi, Renato

    2016-07-01

    An active capillary plasma ionization (ACI) source was coupled to a handheld mass spectrometer (Mini 10.5; Aston Labs, West Lafayette, IN, USA) and applied to the direct gas-phase detection and quantification of chemical warfare agent (CWA) related chemicals. Complementing the discontinuous atmospheric pressure interface (DAPI) of the Mini 10.5 mass spectrometer with an additional membrane pump, a quasi-continuous sample introduction through the ACI source was achieved. Nerve agent simulants (three dialkyl alkylphosphonates, a dialkyl phosporamidate, and the pesticide dichlorvos) were detected at low gas-phase concentrations with limits of detection ranging from 1.0 μg/m3 to 6.3 μg/m3. Our results demonstrate a sensitivity enhancement for portable MS-instrumentation by using an ACI source, enabling direct, quantitative measurements of volatile organic compounds. Due to its high sensitivity, selectivity, low power consumption (<80 W) and weight (<13 kg), this instrumentation has the potential for direct on-site CWA detection as required by military or civil protection.

  3. Direct and Sensitive Detection of CWA Simulants by Active Capillary Plasma Ionization Coupled to a Handheld Ion Trap Mass Spectrometer.

    Science.gov (United States)

    Wolf, Jan-Christoph; Etter, Raphael; Schaer, Martin; Siegenthaler, Peter; Zenobi, Renato

    2016-07-01

    An active capillary plasma ionization (ACI) source was coupled to a handheld mass spectrometer (Mini 10.5; Aston Labs, West Lafayette, IN, USA) and applied to the direct gas-phase detection and quantification of chemical warfare agent (CWA) related chemicals. Complementing the discontinuous atmospheric pressure interface (DAPI) of the Mini 10.5 mass spectrometer with an additional membrane pump, a quasi-continuous sample introduction through the ACI source was achieved. Nerve agent simulants (three dialkyl alkylphosphonates, a dialkyl phosporamidate, and the pesticide dichlorvos) were detected at low gas-phase concentrations with limits of detection ranging from 1.0 μg/m(3) to 6.3 μg/m(3). Our results demonstrate a sensitivity enhancement for portable MS-instrumentation by using an ACI source, enabling direct, quantitative measurements of volatile organic compounds. Due to its high sensitivity, selectivity, low power consumption (<80 W) and weight (<13 kg), this instrumentation has the potential for direct on-site CWA detection as required by military or civil protection. Graphical Abstract ᅟ.

  4. Quantification of Trace Amounts of Impurities in High Purity Cobalt by High Resolution Inductively Coupled Plasma Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    Hua Lin XIE; Xi Du NIE; You Gen TANG

    2006-01-01

    An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to thc presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%- 111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.

  5. Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    XIE Hualin; HUANG Kelong; NIE Xidu; TANG Yougen

    2007-01-01

    An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn,Sb, Ba, Pt, Au, and Pb) in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects because of the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 μg.g-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.

  6. Bioimaging of metals in brain tissue by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and metallomics.

    Science.gov (United States)

    Becker, J Sabine; Matusch, Andreas; Palm, Christoph; Salber, Dagmar; Morton, Kathryn A; Becker, J Susanne

    2010-02-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been developed and established as an emerging technique in the generation of quantitative images of metal distributions in thin tissue sections of brain samples (such as human, rat and mouse brain), with applications in research related to neurodegenerative disorders. A new analytical protocol is described which includes sample preparation by cryo-cutting of thin tissue sections and matrix-matched laboratory standards, mass spectrometric measurements, data acquisition, and quantitative analysis. Specific examples of the bioimaging of metal distributions in normal rodent brains are provided. Differences to the normal were assessed in a Parkinson's disease and a stroke brain model. Furthermore, changes during normal aging were studied. Powerful analytical techniques are also required for the determination and characterization of metal-containing proteins within a large pool of proteins, e.g., after denaturing or non-denaturing electrophoretic separation of proteins in one-dimensional and two-dimensional gels. LA-ICP-MS can be employed to detect metalloproteins in protein bands or spots separated after gel electrophoresis. MALDI-MS can then be used to identify specific metal-containing proteins in these bands or spots. The combination of these techniques is described in the second section.

  7. Determination of cyclovirobuxine D in human plasma by liquid chromatography tandem mass spectrometry and application in a pharmacokinetic study

    Directory of Open Access Journals (Sweden)

    Ling-li Mu

    2011-10-01

    Full Text Available A sensitive and reliable method based on liquid chromatography tandem mass spectrometry (LC–MS/MS for the quantitation of cyclovirobuxine D in human plasma has been developed and validated. Sample preparation by solid phase extraction was followed by separation on a CN column with a mobile phase of methanol–water (95:5, v/v containing 0.2% formic acid. Mass spectrometric detection in the positive ion mode was carried out by selected reaction monitoring (SRM of the transitions at m/z 403.0→372.0 for cyclovirobuxine D and m/z 325.0→234.0 for citalopram (internal standard. The method was linear in the range 10–200 ng/L with LLOQ of 10 ng/L, recovery >85%, and no significant matrix effects. Intra- and inter-day precisions were all <9% with accuracies of 94.0–104.8%. The method was successfully applied to a pharmacokinetic study involving a single oral administration of a 2 mg cyclovirobuxine D tablet to twenty-two healthy Chinese volunteers.

  8. Identification of metabolites of Radix Paeoniae Alba extract in rat bile, plasma and urine by ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Zheng-Wei Chen; Ling Tong; Shu-Ming Li; Dong-Xiang Li; Ying Zhang; Shui-Ping Zhou; Yong-Hong Zhu; He Sun

    2014-01-01

    Ultra-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF/MS) was developed to identify the absorbed parent components and metabolites in rat bile, plasma and urine after oral administration of Radix Paeoniae Alba extract (RPAE). A total of 65 compounds were detected in rat bile, plasma and urine samples, including 11 parent compounds and 54 metabolites. The results indicated that glucuronidation, hydroxylation and methylation were the major metabolic pathways of the components of RPAE. Furthermore, the results of this work demonstrated that UPLC-Q-TOF/MS combined with MetaboLynx™ software and mass defect filtering (MDF) could provide unique high throughput capabilities for drug metabolism study, with excellent MS mass accuracy and enhanced MSE data acquisition. With the MSE technique, both precursor and fragment mass spectra can be simultaneously acquired by alternating between high and low collision energy during a single chromatographic run.

  9. Strategies for the analysis of coal by laser ablation inductively coupled plasma mass spectroscopy.

    Science.gov (United States)

    Kleiber, L; Fink, H; Niessner, R; Panne, U

    2002-09-01

    The potential of laser ablation inductively coupled mass spectrometry (LA-ICP-MS) was investigated for the inorganic characterization of different coal samples pressed into pellets. Reference analysis was performed by microwave-assisted digestion of the ground samples followed by ICP-MS analysis of the resulting solutions. Two different laser ablation sampling procedures were compared. For continuous sampling, three sites of the pellet were sampled for approximately one minute, whereas for sequential sampling 15 sites were sampled for two seconds, respectively. The qualitative results of the two procedures were equivalent, but continuous sampling allowed faster analysis and better precision (RSD about 10%) than sequential sampling (RSD 10-20%). Different normalization procedures with internal and extrinsic standards were investigated and allowed a quantitative determination of Al, Ti, Zn, Ni, and V with measurement uncertainties below 10% and Fe, Si, and Sn with measurement uncertainties below 20%.

  10. Strategies for the analysis of coal by laser ablation inductively coupled plasma mass spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kleiber, L.; Fink, H.; Niessner, R.; Panne, U. [Institute of Hydrochemistry, Technical University of Munich, Marchioninistr. 17, 81377 Munich (Germany)

    2002-09-01

    The potential of laser ablation inductively coupled mass spectrometry (LA-ICP-MS) was investigated for the inorganic characterization of different coal samples pressed into pellets. Reference analysis was performed by microwave-assisted digestion of the ground samples followed by ICP-MS analysis of the resulting solutions. Two different laser ablation sampling procedures were compared. For continuous sampling, three sites of the pellet were sampled for approximately one minute, whereas for sequential sampling 15 sites were sampled for two seconds, respectively. The qualitative results of the two procedures were equivalent, but continuous sampling allowed faster analysis and better precision (RSD about 10%) than sequential sampling (RSD 10-20%). Different normalization procedures with internal and extrinsic standards were investigated and allowed a quantitative determination of Al, Ti, Zn, Ni, and V with measurement uncertainties below 10% and Fe, Si, and Sn with measurement uncertainties below 20%. (orig.)

  11. Alpha heating and isotopic mass effects in JET plasmas with sawteeth

    Energy Technology Data Exchange (ETDEWEB)

    Budny, R. V. [Princeton Plasma Physics Lab. (PPPL), Princeton, NJ (United States); Team, JET [EUROfusion Consortium, JET, Culham Science Centre, Abingdon, OX14 3DB, UK

    2016-02-09

    The alpha heating experiment in the Joint European Torus (JET) 1997 DTE1 campaign is re-examined. Several effects correlated with tritium content and thermal hydrogenic isotopic mass < A> weaken the conclusion that alpha heating was clearly observed. These effects delayed the occurrence of significant sawtooth crashes allowing the electron and ion temperatures T e and T i to achieve higher values. Under otherwise equal circumstances T e and T i were typically higher for discharges with higher < A >, and significant scaling of T i, T e, and total stored energy with < A > were observed. The higher T i led to increased ion–electron heating rates with magnitudes comparable to those computed for alpha electron heating. Rates of other heating/loss processes also had comparable magnitudes. Simulations of T e assuming the observed scaling of T i are qualitatively consistent with the measured profiles, without invoking alpha heating

  12. Prevalence of the angiotensin I converting enzyme insertion/deletion polymorphism, plasma angiotensin converting enzyme activity, and left ventricular mass in a normotensive Chilean population.

    Science.gov (United States)

    Jalil, J E; Piddo, A M; Cordova, S; Chamorro, G; Braun, S; Jalil, R; Vega, J; Jadue'P, L; Lavandero, S; Lastra, P

    1999-07-01

    The aim of this study was to estimate the prevalence of the different alleles of the angiotensin converting enzyme (ACE) gene insertion/deletion (I/D) polymorphism and associated plasma ACE activity, as well as cardiac echocardiographic structure, in a healthy Chilean population. We selected 117 healthy normotensive subjects (aged 45 to 60 years, middle socioeconomic status, nonobese, and nondiabetic) from a population-based study concerning the prevalence of risk factors for chronic diseases (Conjunto de Acciones Para la Reducción Multifactorial de las Enfermedades no Transmisibles [CARMEN]). The frequencies of the I and D alleles were 0.57 and 0.43, respectively. Mean plasma ACE activity was 15.3 +/- 3.9 U/mL. Compared with subjects with the II genotype, plasma ACE activity was significantly higher in subjects with the ID and DD genotypes with no difference between them. No correlation was observed between blood pressure and plasma ACE activity. Among the three different genotypes there was no difference in left ventricular (LV) dimensions or in LV mass. No correlation between plasma ACE activity and LV mass was observed for either gender or different genotypes. Multivariate linear regression analysis using LV mass and LV mass index as dependent variables showed independent effects (P < .05) for gender (higher LV mass in men) and diastolic blood pressure, but not for the DD genotype. In conclusion, in this population, the presence of the D allele on the ACE gene determined higher circulating ACE activity. However, in this normotensive healthy population, male gender and diastolic blood pressure, but not the presence of the D allele, were associated with increased LV mass.

  13. Determination of multiple human arsenic metabolites employing high performance liquid chromatography inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Stice, Szabina; Liu, Guangliang; Matulis, Shannon; Boise, Lawrence H.; Cai, Yong

    2016-01-01

    During the metabolism of different arsenic-containing compounds in human, a variety of metabolites are produced with significantly varying toxicities. Currently available analytical methods can only detect a limited number of human metabolites in biological samples during one run due to their diverse characteristics. In addition, co-elution of species is often unnoticeable with most detection techniques leading to inaccurate metabolic profiles and assessment of toxicity. A high performance liquid chromatography inductively coupled mass spectrometry (HPLC-ICP-MS) method was developed that can identify thirteen common arsenic metabolites possibly present in human with special attention dedicated to thiolated or thiol conjugated arsenicals. The thirteen species included in this study are arsenite (AsIII), arsino-glutathione (As(GS)3), arsenate (AsV), monomethylarsonous acid (MMAIII), monomethylarsino-glutathione (MMAIII(GS)2), monomethylarsonic acid (MMAV), dimethylarsinous acid (DMAIII (from DMAIIII)), S-(dimethylarsinic)cysteine (DMAIII(Cys)), dimethylarsino-glutathione (DMAIII(GS)), dimethylarsinic acid (DMAV), dimethylmonothioarsinic acid (DMMTAV), dimethyldithioarsinic acid (DMDTAV), dimethylarsinothioyl glutathione (DMMTAV(GS)). The developed method was applied for the analysis of cancer cells that were incubated with Darinaparsin (DMAIII(GS)), a novel chemotherapeutic agent for refractory malignancies, and the arsenic metabolic profile obtained was compared to results using a previously developed method. This method provides a useful analytical tool which is much needed in unequivocally identifying the arsenicals formed during the metabolism of environmental arsenic exposure or therapeutic arsenic administration. PMID:26708625

  14. Expansion of a shock plasma in the accelerating field of a parallel-plate capacitor in a time-of-flight mass spectrometer

    Science.gov (United States)

    Semkin, N. D.; Pomel'nikov, R. A.; Telegin, A. M.

    2014-05-01

    We have solved the problem of expansion of a multicomponent shock plasma (initiated by an impact of a fast microprojectile against a solid target) to vacuum in the electric field of a parallel-plate capacitor. The results of calculations can be used in the development of a dust impact mass spectrometer for studying the elemental composition of micrometeorites.

  15. Physicochemical characterization of titanium dioxide pigments using various techniques for size determination and asymmetric flow field flow fractionation hyphenated with inductively coupled plasma mass spectrometry

    NARCIS (Netherlands)

    Helsper, J.P.F.G.; Peters, R.J.B.; Bemmel, M.E.M. van; Rivera, Z.E.H.; Wagner, S.; Kammer, F. von der; Tromp, P.C.; Hofmann, T.; Weigel, S.

    2016-01-01

    Seven commercial titanium dioxide pigments and two other well-defined TiO2 materials (TiMs) were physicochemically characterised using asymmetric flow field flow fractionation (aF4) for separation, various techniques to determine size distribution and inductively coupled plasma mass spectrometry (IC

  16. No genetic footprints of the fat mass and obesity associated (FTO) gene in human plasma 1H CPMG NMR metabolic profiles

    DEFF Research Database (Denmark)

    Kjeldahl, Karin; Rasmussen, Morten Arendt; Hasselbalch, Ann Louise

    2014-01-01

    In this paper it was investigated if any genotypic footprints from the fat mass and obesity associated (FTO) SNP could be found in 600 MHz 1H CPMG NMR profiles of around 1,000 human plasma samples from healthy Danish twins. The problem was addressed with a combination of univariate and multivariate...

  17. Liquid chromatography-tandem mass spectrometric assay for the tyrosine kinase inhibitor afatinib in mouse plasma using salting-out liquid-liquid extraction

    NARCIS (Netherlands)

    Sparidans, Rolf W; van Hoppe, Stephanie; Rood, Johannes J M; Schinkel, Alfred H; Schellens, Jan H M; Beijnen, Jos H

    2016-01-01

    A quantitative bioanalytical liquid chromatography-tandem mass spectrometric (LC-MS/MS) assay for afatinib, an irreversible inhibitor of the ErbB (erythroblastic leukemia viral oncogene homolog) tyrosine kinase family, was developed and validated. Plasma samples were pre-treated using salting-out as

  18. Determination of telmisartan in human blood plasma: Part II: Liquid chromatography-tandem mass spectrometry method development, comparison to immunoassay and pharmacokinetic study

    NARCIS (Netherlands)

    Hempen, C.M.; Gläsle-Schwarz, Liane; Kunz, Ulrich; Karst, U.

    2006-01-01

    A new liquid chromatography/atmospheric pressure chemical ionization-tandem mass spectrometry (LC/APCI-MS/MS) method with on-line sample clean-up for the determination of telmisartan in human blood plasma is presented. This technique is compared to a previously introduced enzyme-linked immunosorbent

  19. Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2013-01-01

    A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 mL) i...

  20. Determination of Total Arsenic and Speciation in Apple Juice by Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry: An Experiment for the Analytical Chemistry Laboratory

    Science.gov (United States)

    He, Ping; Colon, Luis A.; Aga, Diana S.

    2016-01-01

    A two-part laboratory experiment was designed for upper-level analytical chemistry students to provide hands-on experience in the use of high performance liquid chromatography (HPLC) for separation and inductively coupled plasma mass spectrometry (ICP-MS) for detection. In the first part of the experiment, the students analyze total arsenic in…

  1. High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

    NARCIS (Netherlands)

    Hennekam, Rick|info:eu-repo/dai/nl/357286081; Jilbert, Tom|info:eu-repo/dai/nl/304835714; Mason, Paul R D|info:eu-repo/dai/nl/304829331; de Lange, Gert J.|info:eu-repo/dai/nl/073930962; Reichart, Gert Jan|info:eu-repo/dai/nl/165599081

    2015-01-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (μm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

  2. High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

    NARCIS (Netherlands)

    Hennekam, R.; Jilbert, T.; de Lange, G.J.; Reichart, G.J.

    2015-01-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (µm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

  3. Online Coupling of Flow-Field Flow Fractionation and Single Particle Inductively Coupled Plasma-Mass Spectrometry: Characterization of Nanoparticle Surface Coating Thickness and Aggregation State

    Science.gov (United States)

    Surface coating thickness and aggregation state have strong influence on the environmental fate, transport, and toxicity of engineered nanomaterials. In this study, flow-field flow fractionation coupled on-line with single particle inductively coupled plasma-mass spectrometry i...

  4. Comparison of an ultrasonic nebulizer with a cross-flow nebulizer for selenium speciation by ion-chromatography and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Jons, O.

    2000-01-01

    The purpose of this work was to compare an ultrasonic nebulizer (USN) with a cross-flow nebulizer (CFN) for selenium speciation with inductively coupled plasma mass spectrometry (ICP-MS) detection. The influence of instrumental parameters as well as composition of the solvent on the selenium...

  5. No evidence for genome-wide interactions on plasma fibrinogen by smoking, alcohol consumption and body mass index : Results from meta-analyses of 80,607 subjects

    NARCIS (Netherlands)

    J. Baumert (Jens); J. Huang (Jian); B. McKnight (Barbara); M. Sabater-Lleal (Maria); M. Steri (Maristella); A.Y. Chu (Audrey); S. Trompet (Stella); Lopez, L.M. (Lorna M.); Fornage, M. (Myriam); A. Teumer (Alexander); W. Tang (Weihong); A.R. Rudnicka (Alicja); A. Mälarstig (Anders); J.J. Hottenga (Jouke Jan); M. Kavousi (Maryam); J. Lahti (Jari); T. Tanaka (Toshiko); C. Hayward (Caroline); J.E. Huffman (Jennifer); P.-E. Morange (P.); L.M. Rose (Lynda); S. Basu (Saonli); A. Rumley (Ann); D.J. Stott (David. J.); B.M. Buckley (Brendan M.); A.J. de Craen (Anton); S. Sanna (Serena); G. Masala (Giovanna); R. Biffar (Reiner); G. Homuth (Georg); A. Silveira (Angela); B. Sennblad (Bengt); A. Goel (Anuj); H. Watkins (Hugh); M. Müller-Nurasyid (Martina); Rückerl, R. (Regina); K.D. Taylor (Kent); Chen, M.-H. (Ming-Huei); E.J.C. de Geus (Eco); A. Hofman (Albert); J.C.M. Witteman (Jacqueline); M.P.M. de Maat (Moniek); A. Palotie (Aarno); G. Davies (Gail); D.S. Siscovick (David); I. Kolcic (Ivana); S.H. Wild (Sarah); Song, J. (Jaejoon); W.L. McArdle (Wendy); I. Ford (Ian); N. Sattar (Naveed); D. Schlessinger (David); A. Grotevendt (Anne); M. Franzosi; Illig, T. (Thomas); M. Waldenberger (Melanie); T. Lumley (Thomas); G.H. Tofler (Geoffrey); G.A.H.M. Willemsen (Gonneke); A.G. Uitterlinden (André); F. Rivadeneira Ramirez (Fernando); K. Räikkönen (Katri); D.I. Chasman (Daniel); A.R. Folsom (Aaron); G.D.O. Lowe (Gordon); R.G.J. Westendorp (Rudi); P.E. Slagboom (Eline); F. Cucca (Francesco); H. Wallaschofski (Henri); R.J. Strawbridge (Rona); U. Seedorf (Udo); W. Koenig (Wolfgang); J.C. Bis (Joshua); K. Mukamal (Kenneth); Van Dongen, J. (Jenny); E. Widen (Elisabeth); O.H. Franco (Oscar); J.M. Starr (John); K.Y. Liu; L. Ferrucci (Luigi); O. Polasek (Ozren); J.F. Wilson (James F); T. Oudot-Mellakh (Tiphaine); H. Campbell (Harry); P. Navarro (Pau); S. Bandinelli (Stefania); Eriksson, J. (Johan); D.I. Boomsma (Dorret); A. Dehghan (Abbas); R. Clarke (Robert); A. Hamsten (Anders); Boerwinkle, E. (Eric); J.W. Jukema (Jan Wouter); S. Naitza (Silvia); P.M. Ridker (Paul); H. Völzke (Henry); Deary, I.J. (Ian J.); A. Reiner (Alexander); D.-A. Tregouet (David-Alexandre); C.J. O'Donnell (Christopher); D.P. Strachan (David); A. Peters (Annette); Smith, N.L. (Nicholas L.)

    2014-01-01

    textabstractPlasma fibrinogen is an acute phase protein playing an important role in the blood coagulation cascade having strong associations with smoking, alcohol consumption and body mass index (BMI). Genome-wide association studies (GWAS) have identified a variety of gene regions associated with

  6. Determination of levetiracetam in human plasma by liquid chromatography/electrospray tandem mass spectrometry and its application to bioequivalence studies.

    Science.gov (United States)

    Jain, Deepak S; Subbaiah, Gunta; Sanyal, Mallika; Pal, Usha; Shrivastav, Pranav S

    2006-01-01

    The first liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for the determination of levetiracetam, an antiepileptic drug, in human plasma is described. The plasma filtrate obtained after solid-phase extraction (SPE), using a polymer-based, hydrophilic-lipophilic balanced (HLB) cartridge, was submitted directly to a short column LC/MS/MS assay. There was no significant matrix effect on the analysis. For validation of the method, the recovery of the free analytes was compared to that from an optimized extraction method, and the analyte stability was examined under conditions mimicking sample storage, handling, and analytical procedures. The extraction procedure yielded extremely clean extracts with a recovery of 79.95% and 89.02% for levetiracetam and the internal standard (IS), respectively. The intra-assay and inter-assay precision for the samples at the lower limit of quantitation (LLOQ) were 6.33 and 6.82%, respectively. The calibration curves were linear for the dynamic range of 0.5 to 50 microg/mL with a correlation coefficient r >/= 0.9971. The intra-assay accuracy at LLOQ, LQC, MQC, and HQC levels ranged from 81.60 to 95.40, 93.00 to 103.47, 95.97 to 104.09, and 91.15 to 95.18%, respectively, while the inter-assay accuracy at LLOQ, LQC, MQC and HQC levels varied from 80.20 to 95.40, 88.53 to 107.53, 95.97 to 108.45, and 91.15 to 112.70%, respectively. The method is rugged and fast with a total instrumental run time of 2 min. The method was successfully applied for bioequivalence studies in human subject samples after oral administration of 1000 mg immediate release (IR) formulations.

  7. A high-efficiency cross-flow micronebulizer interface for capillary electrophoresis and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Li, J; Umemura, T; Odake, T; Tsunoda, K

    2001-12-15

    A pneumatic nebulizer interface for capillary electrophoresis (CE) and inductively coupled plasma mass spectrometry (ICPMS) is reported. The interface is constructed using a high-efficiency cross-flow micronebulizer (HECFMN) and has the following features. (1) Makeup solutions can be fed to the interface by nebulizer self-aspiration and liquid gravity pressurization. (2) The liquid dead volume of the interface is approximately 65 nL, much smaller than those (200-2500 nL) reported for other interfaces. (3) The interface can be stably operated at a liquid flow rate down to 5 microL/min with a high analyte transport efficiency up to 95% to the plasma and (4) does not induce noticeable laminar flow in the CE capillary at typical nebulizer gas flow rates of 0.8-1.2 L/min. Because of these features, baseline resolution of 10 lanthanides with a CE-ICPMS system using the HECFMN interface is achieved, and detection limits and peak asymmetry are 0.05-1 microg/L and 0.93-1.23, respectively, improved significantly over those reported previously for a CE-ICPMS system using a high-efficiency nebulizer interface. Peak precision for the 10 lanthanides is in the range of 6.2-12.3% RSD (N = 5). Peak widths are from 9.1 s for 139La to 17.9 s for 175Lu. The effects of nebulizer gas flow rate, makeup solution flow rate, and spray chamber volume on CE-ICPMS signal intensity and separation are also evaluated for the HECFMN interface by the separation of Cr3+ and Cr2O7(2-).

  8. Trace element biomonitoring in hair of school children from a polluted area by sector field inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Drobyshev, Evgenii J; Solovyev, Nikolay D; Ivanenko, Natalya B; Kombarova, Maria Yu; Ganeev, Alexander A

    2017-01-01

    In the current study, a biomonitoring of 18 hair trace elements (Al, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Ni, Pb, Se, V, Zn, Ca, Na and P) in school children from Leningradskaya Oblast' is reported. A case group, residing in a proximity to the toxic waste disposal grounds (Krasniy Bor), has been assessed vs. controls from a non-urban settlement Seltso. In total, 166 hair samples were analysed using double focusing sector field inductively coupled plasma mass spectrometry after microwave-assisted sample digestion with nitric acid. For the determination of Ca, Na and P inductively coupled plasma optical emission spectrometry was employed. For the validation, a reference material and spiked hair samples were analysed. The data obtained was processed using parametric statistics and factor analysis. Determined concentrations of trace elements were in agreement with the previously published results on chemically polluted areas. In the case group, linear correlations between Al, Cr, Cu, Fe, Ni and V were observed. Also, these metals correlated to selenium hair content in the case group. Additionally, a correlation between hair Se and P was observed in the case subjects. Several gender differences in trace content were observed within each group. However, no age- or body index-related difference was found. The obtained results show that closely located waste disposal grounds intensifies trace element exposure in school children of Krasniy Bor. However, judging from rather high values for the controls, total environmental status of the region seems to be unstable, so additional monitoring and chemical safety measures are required. Copyright © 2016 Elsevier GmbH. All rights reserved.

  9. Quantitation of S-Adenosylmethionine and S-Adenosylhomocysteine in Plasma Using Liquid Chromatography-Electrospray Tandem Mass Spectrometry.

    Science.gov (United States)

    Arning, Erland; Bottiglieri, Teodoro

    2016-01-01

    We describe a simple stable isotope dilution method for accurate determination of S-adenosylmethionine (SAM) and S-adenosylhomocysteine (SAH) in plasma as a diagnostic test. SAM and SAH are key metabolic intermediates of methionine metabolism and the methylation cycle. Determination of SAM and SAH in plasma was performed by high performance liquid chromatography coupled with electrospray positive ionization tandem mass spectrometry (HPLC-ESI-MS/MS). Calibrators (SAM and SAH) and internal standards ((2)H3-SAM and (2)H4-SAH) were included in each analytical run for calibration. Sample preparation involved combining 20 μL sample with 180 μL of internal standard solution consisting of heavy isotope labeled internal standards in mobile phase A and filtering by ultracentrifugation through a 10 kd MW cutoff membrane. Sample filtrate (3 μL) was injected by a Shimadzu Nexera LC System interfaced with a 5500 QTRAP(®) (AB Sciex). Chromatographic separation was achieved on a 250 mm × 2.0 mm EA:faast column from Phenomenex. Samples were eluted at a flow rate of 0.20 mL/min with a binary gradient with a total run time of 10 min. The source operated in positive ion mode at an ion spray voltage of +5000 V. SAM and SAH resolved by a gradient to 100 % methanol with retention times of 6.0 and 5.7 min, respectively. The observed m/z values of the fragment ions were m/z 399 → 250 for SAM, m/z 385 → 136 for SAH, m/z 402 → 250 for (2)H3-SAM, m/z 203 → 46. The calibration curve was linear over the ranges of 12.5-5000 nmol/L for SAM and SAH.

  10. High resolution mass spectrometry coupled with multivariate data analysis revealing plasma lipidomic alteration in ovarian cancer in Asian women.

    Science.gov (United States)

    Zhang, Yangyang; Liu, Yingying; Li, Lin; Wei, Jinchao; Xiong, Shaoxiang; Zhao, Zhenwen

    2016-04-01

    Ovarian cancer (OC) is the most common cause of death from gynecologic malignancies in women. The identification of reliable diagnostic biomarkers for the early detection of this deadly disease is critical for reducing the mortality rate of OC. Plasma lysophosphatidic acid (LPA) levels were increased from OC patients vs. healthy controls. Therefore, lipidomics may represent an excellent developing prospect for the discovery of diagnostic biomarkers of OC. In this study, a nontargeted lipidomics approach based on ultra performance liquid chromatography-electrospray ionization-QTOF-mass spectrometry (UPLC-ESI-QTOF-MS) combined with multivariate data analysis, including principal component analysis (PCA) and (orthogonal) partial least squared discriminant analysis [(O)PLS-DA] was applied for the investigation of potential diagnostic biomarkers in plasma of OC patients. Patients with OC could be distinguished from healthy individuals and patients with benign gynecological tumor disease by this method, which shows a significant lipid perturbation in this disease. With the assistance of high resolution and high accuracy of MS and MS/MS data, the potential markers including lysophosphatidylcholines (LPCs), phosphatidylcholines (PCs) and triacylglycerols (TGs) with specific fatty acid chains, were identified. Interestingly, LPCs were up-regulated and PCs and TGs were down-regulated, compared OC group with benign tumor and normal control groups, and the glycerophospholipid metabolism emerged as a key pathway, in particular, the phospholipase A2 (PLA2) enzyme activity, that was disregulated in the disease. This study may provide new insight into underlying mechanisms for OC and proves that MS-based lipidomics is a powerful method in discovering new potential clinical biomarkers for diseases. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Liquid Chromatography Tandem Mass Spectrometry Method for Quantification of Solifenacin in Human Plasma and its Application to Bioequivalence Study

    Directory of Open Access Journals (Sweden)

    Nishant Paliwal

    2013-06-01

    Full Text Available A hasty, specific and robust assay based on liquid-liquid extraction and liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI MS-MS has been developed and validated for the quantitative analysis of Solifenacin ( a drug used for urinary incontinence in human plasma using Solifenacin D5 as internal standard (ISTD. The precursor to product ion transitions of m/z 363.20/110.10 and m/z 368.14/110.20 were used to measure the analyte and the ISTD, respectively. The method was validated in terms of selectivity, matrix effect, sensitivity, linearity, precision and accuracy, various stabilities (standard stock solution stability in refrigerator and at room temperature, stock dilution stability at refrigerator and room temperature, auto sampler stability, freeze thaw stability, long term stability- 65 o C ± 10o C & long term stability- 22 o C ± 5°C, reagent stability, bench top stability, dry extract stability, wet extract stability in refrigerator, effect of potentially interfering drugs, dilution integrity, recovery, lon suppression through infusion, and blood Stability. The mean percentage recovery of Solifenacin and the internal standard was 65.39 ± 3.646% and 66.24 ± 2.209% respectively. The assay exhibited a linear dynamic range of 0.200 to 30.361 ng mL-1. The RSD % of intra-day and inter-day assay was ≤15%. The application of this assay was demonstrated in a bioequivalence study and will be ideal for clinical pharmacokinetic studies in study population with as lower as 0.200 ng mL-1 analytical sensitivity and as little as 300 μL plasma sample.

  12. New ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of irbesartan in human plasma

    Directory of Open Access Journals (Sweden)

    Tanveer A. Wani

    2015-09-01

    Full Text Available With the objective of reducing analysis time and maintaining good efficiency, there has been substantial focus on high-speed chromatographic separations and ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS is a preeminent analytical tool for rapid biomedical analysis. In this study a simple, rapid, sensitive, and specific ultra-performance liquid chromatography-MS/MS method was developed and validated for quantification of the angiotensin II receptor antagonist, irbesartan (IRB, in human plasma. After a simple protein precipitation using methanol and acetonitrile, IRB and internal standard (IS telmisartan were separated on Acquity UPLC BEH C18 column (50 mm × 2.1 mm, i.d. 1.7 μm, Waters, Milford, MA, USA using a mobile phase consisted of acetonitrile: methanol: 10 mM ammonium acetate (70: 15: 15 v/v/v with a flow rate of 0.4 mL/min and detected MS/MS in negative ion mode. The ion transitions recorded in multiple reaction monitoring mode were m/z 427.2→193.08 for IRB and m/z 513.2→469.3 for IS. The assay exhibited a linear dynamic range of 2–500 ng/mL for IRB in human plasma with good correlation coefficient of (0.995 and with a lower limit of quantitation of 2 ng/mL. The intra- and interassay precisions were satisfactory; the relative standard deviations did not exceed 9.91%. The proposed UPLC-MS/MS method is simple, rapid, and highly sensitive, and hence it could be reliable for pharmacokinetic and toxicokinetic study in both animals and humans.

  13. Optical diagnostics and mass spectrometry on the afterglow of an atmospheric pressure Ar/O$_2$ radiofrequency plasma used for polymer surface treatment

    CERN Document Server

    Duluard, Corinne Y; Hubert, Julie; Reniers, François

    2016-01-01

    In the context of polymer surface treatment, the afterglow of an atmospheric pressure Ar/O$_2$ radiofrequency plasma is characterized by optical emission spectroscopy, laser induced fluorescence and mass spectrometry. The influence of the O$_2$ gas flow rate and the source power on the plasma properties (gas temperature, Ar excitation temperature, relative concentrations of O atoms and OH radicals) are evaluated. We show that for plasma torch-to-substrate distances lower than 6 mm, the afterglow creates a protective atmosphere, thus the plasma gas composition interacting with the substrate is well controlled. For higher distances, the influence of ambient air can no longer be neglected and gradients in Ar, O$_2$ and N$_2$ concentrations are measured as a function of axial and vertical position.

  14. Evaluation of capillary supercritical fluid chromatography with mass spectrometric detection for the analysis of a drug (mebeverine) in a dog plasma matrix.

    Science.gov (United States)

    Pinkston, J D; Venkatramani, C J; Tulich, L J; Bowling, D J; Wehmeyer, K R

    1993-12-22

    Supercritical fluid chromatography with mass spectrometric detection was evaluated as a technique for the analysis of drugs in biological fluids. Dog plasma was spiked with a model drug, mebeverine, and with a deuterium-labeled analog of mebeverine. The spiked plasma was prepared for analysis by solid-phase extraction on octadecylsilane cartridges. Mebeverine levels in the spiked dog plasma samples were determined by interpolation from a standard curve. Accuracy and precision of the analysis were determined within and between days. In general, accuracy was found to be 100 +/- 15% for plasma samples spiked with 6 to 60 ng mebeverine/ml. The relative standard deviation for replicate sample analysis over this concentration range was between 5 and 12.5%.

  15. IgY14 and SuperMix immunoaffinity separations coupled with liquid chromatography-mass spectrometry for human plasma proteomic biomarker discovery

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Tujin; Zhou, Jianying; Gritsenko, Marina A.; Hossain, Mahmud; Camp, David G.; Smith, Richard D.; Qian, Weijun

    2012-02-01

    Interest in the application of advanced proteomics technologies to human blood plasma- or serum-based clinical samples for the purpose of discovering disease biomarkers continues to grow; however, the enormous dynamic range of protein concentrations in these types of samples (often >10 orders of magnitude) represents a significant analytical challenge, particularly for detecting low-abundance candidate biomarkers. In response, immunoaffinity separation methods for depleting multiple high- and moderate-abundance proteins have become key tools for enriching low-abundance proteins and enhancing detection of these proteins in plasma proteomics. Herein, we describe IgY14 and tandem IgY14-Supermix separation methods for removing 14 high-abundance and up to 60 moderate-abundance proteins, respectively, from human blood plasma and highlight their utility when combined with liquid chromatography-tandem mass spectrometry for interrogating the human plasma proteome.

  16. IgY14 and SuperMix immunoaffinity separations coupled with liquid chromatography-mass spectrometry for human plasma proteomics biomarker discovery.

    Science.gov (United States)

    Shi, Tujin; Zhou, Jian-Ying; Gritsenko, Marina A; Hossain, Mahmud; Camp, David G; Smith, Richard D; Qian, Wei-Jun

    2012-02-01

    Interest in the application of advanced proteomics technologies to human blood plasma- or serum-based clinical samples for the purpose of discovering disease biomarkers continues to grow; however, the enormous dynamic range of protein concentrations in these types of samples (often >10 orders of magnitude) represents a significant analytical challenge, particularly for detecting low-abundance candidate biomarkers. In response, immunoaffinity separation methods for depleting multiple high- and moderate-abundance proteins have become key tools for enriching low-abundance proteins and enhancing detection of these proteins in plasma proteomics. Herein, we describe IgY14 and tandem IgY14-Supermix separation methods for removing 14 high-abundance and up to 60 moderate-abundance proteins, respectively, from human blood plasma and highlight their utility when combined with liquid chromatography-tandem mass spectrometry for interrogating the human plasma proteome.

  17. Determination of myrtucommulone from Myrtus communis in human and rat plasma by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Gerbeth, Kathleen; Meins, Jürgen; Werz, Oliver; Schubert-Zsilavecz, Manfred; Abdel-Tawab, Mona

    2011-03-01

    Recent studies revealed that the non-prenylated acylphloroglucinol myrtucommulone (MC) from myrtle ( MYRTUS COMMUNIS) potently suppresses the biosynthesis of eicosanoids by direct inhibition of cyclooxygenase-1, microsomal prostaglandin E2 synthase (mPGES)-1, and 5-lipoxygenase at IC₅₀ values in the range of 1 to 29 µM. Moreover, MC showed potent efficacy in animal models of inflammation after intraperitoneal administration. Since the main prerequisite for therapeutic efficacy is sufficient bioavailability, it is important to evaluate whether the concentrations of MC achieved in plasma coincide with the pharmacological active concentrations determined in vitro. For that reason, a sensitive LC/MS/MS method has been developed and validated for the determination of MC in human plasma. This method is based on liquid-liquid extraction of plasma samples with 20 % ethyl acetate in tert-butyl methyl ether using the structurally related acylphloroglucinol hyperforin as the internal standard. Chromatographic separation was achieved on a Gemini C6 Phenyl column using a mixture of acetonitrile/water (85 : 15 v/v) containing 6 mM ammonium formate in a run time of 15 min at a flow rate of 1 mL/min, a column temperature of 40 °C, and an autosampler temperature of 5 °C. Mass spectrometric quantification was carried out in the negative ion mode using electrospray ionization (ESI) and multiple-reaction monitoring (MRM). The most intense [M-H]⁻ MRM transition at m/z 667.4 → m/z 194.9 was used for quantification of MC and the transition at m/z 535.4 to m/z 383.2 was used to monitor hyperforin. The method was linear in the range of 1-100 ng/mL with r > 0.998, an intra- and inter-day RSD of 1.1-8.4 and 7.1-11.8 %, respectively, and a maximum R. E. of 13.8 % at the lowest concentration level. Moreover, cross validation revealed the suitability of the developed LC/MS method for application in rat studies.

  18. Non-spectral interferences due to the presence of sulfuric acid in inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    García-Poyo, M. Carmen; Grindlay, Guillermo; Gras, Luis [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, P.O. Box 99, 03080 – Alicante (Spain); Loos-Vollebregt, Margaretha T.C. de, E-mail: margaretha.deloos@ugent.be [Delft University of Technology, Faculty of Applied Sciences, Analytical Biotechnology, Julianalaan 67, 2628 BC Delft (Netherlands); Ghent University, Department of Analytical Chemistry, Krijgslaan 281 - S12, 9000 Ghent (Belgium); Mora, Juan, E-mail: juan.mora@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, P.O. Box 99, 03080 – Alicante (Spain)

    2015-03-01

    Results of a systematic study concerning non-spectral interferences from sulfuric acid containing matrices on a large number of elements in inductively coupled plasma–mass spectrometry (ICP-MS) are presented in this work. The signals obtained with sulfuric acid solutions of different concentrations (up to 5% w w{sup −1}) have been compared with the corresponding signals for a 1% w w{sup −1−} nitric acid solution at different experimental conditions (i.e., sample uptake rates, nebulizer gas flows and r.f. powers). The signals observed for {sup 128}Te{sup +}, {sup 78}Se{sup +} and {sup 75}As{sup +} were significantly higher when using sulfuric acid matrices (up to 2.2-fold for {sup 128}Te{sup +} and {sup 78}Se{sup +} and 1.8-fold for {sup 75}As{sup +} in the presence of 5 w w{sup -1} sulfuric acid) for the whole range of experimental conditions tested. This is in agreement with previously reported observations. The signal for {sup 31}P{sup +} is also higher (1.1-fold) in the presence of sulfuric acid. The signal enhancements for {sup 128}Te{sup +}, {sup 78}Se{sup +}, {sup 75}As{sup +} and {sup 31}P{sup +} are explained in relation to an increase in the analyte ion population as a result of charge transfer reactions involving S{sup +} species in the plasma. Theoretical data suggest that Os, Sb, Pt, Ir, Zn and Hg could also be involved in sulfur-based charge transfer reactions, but no experimental evidence has been found. The presence of sulfuric acid gives rise to lower ion signals (about 10–20% lower) for the other nuclides tested, thus indicating the negative matrix effect caused by changes in the amount of analyte loading of the plasma. The elemental composition of a certified low-density polyethylene sample (ERM-EC681K) was determined by ICP-MS after two different sample digestion procedures, one of them including sulfuric acid. Element concentrations were in agreement with the certified values, irrespective of the acids used for the digestion. These

  19. Postprandial metabolomics: A pilot mass spectrometry and NMR study of the human plasma metabolome in response to a challenge meal

    Energy Technology Data Exchange (ETDEWEB)

    Karimpour, Masoumeh; Surowiec, Izabella; Wu, Junfang [Computational Life Science Cluster (CLiC), Department of Chemistry, Umeå University, 90187 Umeå (Sweden); Gouveia-Figueira, Sandra [Computational Life Science Cluster (CLiC), Department of Chemistry, Umeå University, 90187 Umeå (Sweden); Department of Pharmacology and Clinical Neuroscience, Umeå University, Umeå (Sweden); Pinto, Rui [Computational Life Science Cluster (CLiC), Department of Chemistry, Umeå University, 90187 Umeå (Sweden); Bioinformatics Infrastructure for Life Sciences (Sweden); Trygg, Johan [Computational Life Science Cluster (CLiC), Department of Chemistry, Umeå University, 90187 Umeå (Sweden); Zivkovic, Angela M. [Department of Nutrition, University of California, Davis, One Shields Ave, CA 95616 (United States); Nording, Malin L., E-mail: malin.nording@umu.se [Computational Life Science Cluster (CLiC), Department of Chemistry, Umeå University, 90187 Umeå (Sweden)

    2016-02-18

    The study of postprandial metabolism is relevant for understanding metabolic diseases and characterizing personal responses to diet. We combined three analytical platforms – gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS) and nuclear magnetic resonance (NMR) – to validate a multi-platform approach for characterizing individual variation in the postprandial state. We analyzed the postprandial plasma metabolome by introducing, at three occasions, meal challenges on a usual diet, and 1.5 years later, on a modified background diet. The postprandial response was stable over time and largely independent of the background diet as revealed by all three analytical platforms. Coverage of the metabolome between NMR and GC-MS included more polar metabolites detectable only by NMR and more hydrophobic compounds detected by GC-MS. The variability across three separate testing occasions among the identified metabolites was in the range of 1.1–86% for GC-MS and 0.9–42% for NMR in the fasting state at baseline. For the LC-MS analysis, the coefficients of variation of the detected compounds in the fasting state at baseline were in the range of 2–97% for the positive and 4–69% for the negative mode. Multivariate analysis (MVA) of metabolites detected with GC-MS revealed that for both background diets, levels of postprandial amino acids and sugars increased whereas those of fatty acids decreased at 0.5 h after the meal was consumed, reflecting the expected response to the challenge meal. MVA of NMR data revealed increasing postprandial levels of amino acids and other organic acids together with decreasing levels of acetoacetate and 3-hydroxybutanoic acid, also independent of the background diet. Together these data show that the postprandial response to the same challenge meal was stable even though it was tested 1.5 years apart, and that it was largely independent of background diet. This work demonstrates the efficacy of a

  20. Rapid and accurate U-Th dating of ancient carbonates using inductively coupled plasma-quadrupole mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Douville, Eric; Salle, Eline; Frank, Norbert; Pons-Branchu, Edwige; Ayrault, Sophie [Laboratoire des Sciences du Climat et de l' Environnement, LSCE/IPSL, UMR 8212 CNRS-CEA-UVSQ, Domaine du CNRS, F-91198 Gif/Yvette (France); Eisele, Markus [MARUM, University of Bremen, Leobener Str., 28359 Bremen (DE)

    2010-07-01

    Here, the potential for rapid and accurate U-Th dating technique of marine aragonite skeletons (deep-sea corals, Lophelia pertusa) and secondary calcite deposits (speleothems and stalagmites) has been explored using inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS). The analytical procedure includes a largely simplified chemical separation technique for uranium (U) and thorium (Th) using UTEVA resin. The developed technique permits simultaneous quantification of uranium [{sup 238}U] and thorium [{sup 232}Th] concentrations and their respective isotopic composition, required for U-series disequilibrium dating. Up to 50 U-Th dates per day can be achieved through ICP-QMS with {delta}{sup 234}U and {delta}{sup 230}Th reproducibility (2 {sigma}) of 3-4 parts per thousand and 1%, respectively. The high sensitivity ({>=}3.0 x 10{sup 5} cps/ppb) together with low background ({<=}0.5 cps) on each mass between 228 and 236 amu allowed U-Th dating of ancient deep-water corals (15-260 kyr) and stalagmites (30-85 kyr) at precision levels of less than 2%. Consequently, the combination of simplified chemistry using UTEVA with state-of-the-art ICP-QMS isotopic measurements that do not require a U-Th separation step now provides an extremely rapid and low-cost U-series dating technology. The level of precision is most convenient for numerous geochronological applications, such as the determination of climatic influences on ecosystem development and carbonate precipitation. As a first-example application we present ICP-QMS U-Th dates of North Atlantic deep-water coral fragments retrieved in the southeastern Porcupine Seabight (MD01-2463G. Mound Therese), indicating a purely interglacial growth of deep-water corals on so-called carbonate mounds over several climate cycles. (authors)

  1. Measurements of natural carbonate rare earth elements in femtogram quantities by inductive coupled plasma sector field mass spectrometry.

    Science.gov (United States)

    Shen, Chuan-Chou; Wu, Chung-Che; Liu, Yi; Yu, Jimin; Chang, Ching-Chih; Lam, Doan Dinh; Chou, Chien-Ju; Lo, Li; Wei, Kuo-Yen

    2011-09-01

    A rapid and precise standard-bracketing method has been developed for measuring femtogram quantity rare earth element (REE) levels in natural carbonate samples by inductively coupled plasma sector field mass spectrometry that does not require chemical separation steps. A desolvation nebulization system was used to effectively reduce polyatomic interference and enhance sensitivity. REE/Ca ratios are calculated directly from the intensities of the ion beams of (46)Ca, (139)La, (140)Ce, (141)Pr, (146)Nd, (147)Sm, (153)Eu, (160)Gd, (159)Tb, (163)Dy, (165)Ho, (166)Er, (169)Tm, (172)Yb, and (175)Lu using external matrix-matched synthetic standards to correct for instrumental ratio drifting and mass discrimination. A routine measurement time of 3 min is typical for one sample containing 20-40 ppm Ca. Replicate measurements made on natural coral and foraminiferal samples with REE/Ca ratios of 2-242 nmol/mol show that external precisions of 1.9-6.5% (2 RSD) can be achieved with only 10-1000 fg of REEs in 10-20 μg of carbonate. We show that different sources for monthly resolved coral ultratrace REE variability can be distinguished using this method. For natural slow growth-rate carbonate materials, such as sclerosponges, tufa, and speleothems, the high sample throughput, high precision, and high temporal resolution REE records that can be produced with this procedure have the potential to provide valuable time-series records to advance our understanding of paleoclimatic and paleoenvironmental dynamics on different time scales.

  2. Improved analysis of vitamin D metabolites in plasma using liquid chromatography tandem mass spectrometry, and its application to cardiovascular research.

    Science.gov (United States)

    Sandhu, Jatinderpal K; Auluck, Janica; Ng, Leong L; Jones, Donald J L

    2014-06-01

    The accurate and specific measurement of vitamin D is increasingly important for determining the role of vitamin D in the pathogenesis of disease. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS) has increasingly become the analytical modality of choice for the analysis of vitamin D. There are many advantages to using LC/MS/MS, such as high specificity and sensitivity to help distinguish the isomers of vitamin D. This rapid method, modified from a Waters Corporation application note, consists of minimal sample manipulation using liquid-liquid extraction and incorporates an internal standard. The supernatant is dried down and injected onto an ultra-high-performance liquid chromatography/electrospray ionization tandem mass spectrometer. The total analysis time is 10 min per injection, enabling high throughput of samples. This method also incorporates two commercial quality control standards to provide a robust system with acceptable coefficient of variation. The analysis of control and heart failure plasma samples showed significant differences in the levels of vitamin D3 between these two groups; however, in the control group, there were individuals who were vitamin D deficient. Overall, the vitamin D3 levels were higher in control samples than in heart failure individuals. As expected, vitamin D2 levels were not observed in many of the samples analysed. This modified method is quick and incorporates an internal standard to allow for any loss in the extraction procedure. The method also includes quality control samples to enable assay standardization. The assay involves inexpensive pre-sample clean-up, aiding high throughput, which is important in many laboratories.

  3. High plasma cholesteryl ester transfer but not CETP mass predicts incident cardiovascular disease : A nested case control study

    NARCIS (Netherlands)

    Kappelle, Paul J.W.H.; Perton, Frank; Hillege, Hans L.; Dallinga-Thie, Geesje M.; Dullaart, Robin P. F.

    Objective: The relationship of cardiovascular disease (CVD) with plasma cholesteryl ester transfer protein (CETP) levels is controversial. We determined whether plasma cholesteryl ester transfer (CET), reflecting CETP-mediated transfer of cholesteryl esters from endogenous HDL towards apolipoprotein

  4. The role of mass spectrometry in atomic weight determinations.

    Science.gov (United States)

    De Laeter, John R

    2009-01-01

    accurate isotopic measurements. Atomic weights can no longer be regarded as constants of nature, except for the monoisotopic elements whose atomic weights are determined solely by the relative atomic mass of that nuclide. Stable isotope geochemists developed mass spectrometric protocols by the adoption of internationally accepted reference materials for the light elements, to which measurements from various laboratories could be compared. Subsequently, a number of heavy elements such as iron, molybdenum and cadmium have been shown to exhibit isotope fractionation. The magnitude of such isotope fractionation in nature is less than for the light elements, but technological developments, such as multiple collector-inductively coupled plasma-mass spectrometry, have enabled such fractionation effects to be determined. Measurements of the atomic weights of certain elements affect the determination of important fundamental constants such as the Avogadro Constant, the Faraday Constant and the Universal Gas Constant. Heroic efforts have been made to refine the accuracy of the atomic weight of silicon, with the objective of replacing the SI standard of mass--the kilogram--with the Avogadro Constant. Improvements in these fundamental constants in turn affect the set of self-consistent values of other basic constants through a least-squares adjustment methodology. Absolute isotope abundances also enable the Solar System abundances of the s-, r-, and p-process of nucleosynthesis to be accurately determined, thus placing constraints on theories of heavy element nucleosynthesis. Future developments in the science of atomic weight determinations are also examined.

  5. A new ultrafast and high-throughput mass spectrometric approach for the therapeutic drug monitoring of the multi-targeted anti-folate pemetrexed in plasma from lung cancer patients

    NARCIS (Netherlands)

    R.J.W. Meesters (Roland); R. Cornelissen (Robin); R.J. van Klaveren (Rob); R. de Jonge (Robert); E. den Boer (Ethan); J. Lindemans (Jan); T.M. Luider (Theo)

    2010-01-01

    textabstractAn analytical assay has been developed and validated for ultrafast and high-throughput mass spectrometric determination of pemetrexed concentrations in plasma using matrix assisted laser desorption/ionization-triple quadrupole-tandem mass spectrometry. Patient plasma samples spiked with

  6. Speciation of vanadium in oilsand coke and bacterial culture by high performance liquid chromatography inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, X. Sherry [Department of Chemistry, University of Alberta, Edmonton, Alberta T6G 2G2 (Canada); Le, X. Chris [Department of Chemistry, University of Alberta, Edmonton, Alberta T6G 2G2 (Canada); Analytical and Environmental Toxicology, Department of Laboratory Medicine and Pathology, University of Alberta, Edmonton, Alberta T6G 2G3 (Canada)], E-mail: xc.le@ualberta.ca

    2007-10-17

    A simple and sensitive method for the speciation of vanadium(III), (IV), and (V) was developed by using high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICPMS). The EDTA-complexed vanadium species were separated on a strong anion exchange column with an eluent containing 2 mM EDTA, 3% acetonitrile, and 80 mM ammonium bicarbonate at pH 6. Each analysis was complete in 5 min. The detection limits were 0.6, 0.7 and 1.0 {mu}g L{sup -1} for V(III), V(IV), and V(V), respectively. The method was applied to coke pore water samples from an oilsand processing/upgrading site in Fort McMurray, Alberta, Canada and to Shewanella putrefaciens CN32 bacterial cultures incubated with V(V). In the coke pore water samples, V(IV) and V(V) were found to be the major species. For the first time, V(III) was detected in the bacterial cultures incubated with V(V)

  7. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Energy Technology Data Exchange (ETDEWEB)

    Duyck, Christiane Beatrice, E-mail: cbduyck@vm.uff.br [Pontificia Universidade Catolica do Rio de Janeiro (PUC-Rio), R. Marques de Sao Vicente, 225, Gavea, Rio de Janeiro, RJ, 22451-900 (Brazil); Universidade Federal Fluminense (UFF), Campus do Valonguinho, Outeiro de Sao Joao Batista, s/no, 24020-150, Niteroi, RJ (Brazil); Saint' Pierre, Tatiana Dillenburg; Miekeley, Norbert [Pontificia Universidade Catolica do Rio de Janeiro (PUC-Rio), R. Marques de Sao Vicente, 225, Gavea, Rio de Janeiro, RJ, 22451-900 (Brazil); Oliveira da Fonseca, Teresa Cristina; Szatmari, Peter [Centro de Pesquisas Leopoldo A. Miguez de Mello da Petrobras (CENPES), Av. Horacio Macedo, 950, Cidade Universitaria, Rio de Janeiro, RJ, 21941-915 (Brazil)

    2011-05-15

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 {mu}g L{sup -1} and 8 {mu}g L{sup -1}. The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  8. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Science.gov (United States)

    Duyck, Christiane Béatrice; Saint'Pierre, Tatiana Dillenburg; Miekeley, Norbert; da Fonseca, Teresa Cristina Oliveira; Szatmari, Peter

    2011-05-01

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L - 1 and 8 μg L - 1 . The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  9. Analysis of four toxic metals in a single rice seed by matrix solid phase dispersion -inductively coupled plasma mass spectrometry

    Science.gov (United States)

    He, Xiufen; Chen, Lixia; Chen, Xin; Yu, Huamei; Peng, Lixu; Han, Bingjun

    2016-12-01

    Toxic metals in rice pose great risks to human health. Metal bioaccumulation in rice grains is a criterion of breeding. Rice breeding requires a sensitive method to determine metal content in single rice grains to assist the variety selection. In the present study, four toxic metals of arsenic (As), cadmium (Cd), chromium (Cr) and lead (Pb) in a single rice grain were determined by a simple and rapid method. The developed method is based on matrix solid phase dispersion using multi-wall carbon nanotubes (MWCNTs) as dispersing agent and analyzed by inductively coupled plasma mass spectrometry. The experimental parameters were systematically investigated. The limits of detection (LOD) were 5.0, 0.6, 10 and 2.1 ng g‑1 for As, Cd, Cr, and Pb, respectively, with relative standard deviations (n = 6) of microwave digestion. The amount of sample required was reduced approximately 100 fold in comparison with the microwave digestion. The method has a high application potential for other sample matrices and elements with high sensitivity and sample throughput.

  10. Visualizing fossilization using laser ablation-inductively coupled plasma-mass spectrometry maps of trace elements in Late Cretaceous bones

    Science.gov (United States)

    Koenig, A.E.; Rogers, R.R.; Trueman, C.N.

    2009-01-01

    Elemental maps generated by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) provide a previously unavailable high-resolution visualization of the complex physicochemical conditions operating within individual bones during the early stages of diagenesis and fossilization. A selection of LA-ICP-MS maps of bones collected from the Late Cretaceous of Montana (United States) and Madagascar graphically illustrate diverse paths to recrystallization, and reveal unique insights into geochemical aspects of taphonomic history. Some bones show distinct gradients in concentrations of rare earth elements and uranium, with highest concentrations at external bone margins. Others exhibit more intricate patterns of trace element uptake related to bone histology and its control on the flow paths of pore waters. Patterns of element uptake as revealed by LA-ICP-MS maps can be used to guide sampling strategies, and call into question previous studies that hinge upon localized bulk samples of fossilized bone tissue. LA-ICP-MS maps also allow for comparison of recrystallization rates among fossil bones, and afford a novel approach to identifying bones or regions of bones potentially suitable for extracting intact biogeochemical signals. ?? 2009 Geological Society of America.

  11. Effects of Plasma Drag on Low Earth Orbiting Satellites due to Heating of Earth's Atmosphere by Coronal Mass Ejections

    CERN Document Server

    Nwankwo, Victor U J

    2013-01-01

    Solar events, such as coronal mass ejections (CMEs) and solar flares, heat up the upper atmosphere and near-Earth space environment. Due to this heating and expansion of the outer atmosphere by the energetic ultraviolet, X-ray and particles expelled from the sun, the low Earth-Orbiting satellites (LEOS) become vulnerable to an enhanced drag force by the ions and molecules of the expanded atmosphere. Out of various types of perturbations, Earth directed CMEs play the most significant role. They are more frequent and intense during the active (solar maximum) phase of the sun's approximately 11-year cycle. As we are approaching another solar maximum later in 2013, it may be instructive to analyse the effects of the past solar cycles on the orbiting satellites using the archival data of space environment parameters as indicators. In this paper, we compute the plasma drag on a model LEOS due to the atmospheric heating by CMEs and other solar events as a function of the solar parameters. Using the current forecast ...

  12. Direct determination of mercury in cosmetic samples by isotope dilution inductively coupled plasma mass spectrometry after dissolution with formic acid

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Ying; Shi, Zeming; Zong, Qinxia; Wu, Peng; Su, Jing [Sichuan Provincial Key Laboratory of Nuclear Technology in Geology, College of Nuclear Technology and Automation Engineering, Chengdu University of Technology, Chengdu 610059 (China); Liu, Rui, E-mail: liur.ray@gmail.com [Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu 610059 (China)

    2014-02-17

    Graphical abstract: -- Highlights: •Simple, sensitive, and accurate method is established for mercury determination in cosmetics. •The sample preparation procedure is highly simplified. •Isotope dilution efficiently eliminates matrix effect. •First report of using formic acid based method in combination with PVG-ID-ICP MS for mercury quantitation in cosmetics. -- Abstract: A new method was proposed for the accurate determination of mercury in cosmetic samples based on isotopic dilution (ID)-photochemical vapor generation (PVG)-inductively coupled plasma mass spectrometry (ICP MS) measurement. Cosmetic samples were directly dissolved in formic acid solution and subsequently subjected to PVG for the reduction of mercury into vapor species following by ICP MS detection. Therefore, the risks of analyte contamination and loss were avoided. Highly enriched {sup 201}Hg isotopic spike is added to cosmetics and the isotope ratios of {sup 201}Hg/{sup 202}Hg were measured for the quantitation of mercury. With ID calibration, the influences originating from sample matrixes for the determination of mercury in cosmetic samples have been efficiently eliminated. The effects of several experimental parameters, such as the concentration of the formic acid, and the flow rates of carrier gas and sample were investigated. The method provided good reproducibility and the detection limits were found to be 0.6 pg mL{sup −1}. Finally, the developed method was successfully applied for the determination of mercury in six cosmetic samples and a spike test was performed to verify the accuracy of the method.

  13. Rapid and Accurate U-Th Dating of Ancient Carbonates using Inductively Coupled Plasma-Quadrupole Mass Spectrometry

    Science.gov (United States)

    Douville, Eric; Sallé, Eline; Frank, Norbert; Eisele, Markus; Pons-Branchu, Edwige; Ayrault, Sophie

    2010-05-01

    Here, the potential for rapid and accurate U-Th dating technique of marine aragonite skeletons (deep-sea corals, Lophelia pertusa) and secondary calcite deposits (speleothems and stalagmites) has been explored using inductively-coupled plasma-quadrupole mass spectrometry (ICP-QMS). The analytical procedure includes a largely simplified chemical separation technique for uranium (U) and thorium (Th) using UTEVA resin. The developed technique permits simultaneous quantification of uranium [238U] and thorium [232Th] concentrations and their respective isotopic composition, required for U-series disequilibrium dating. Up to 50 U-Th dates per day can be achieved through ICP-QMS with 234U and 230Th reproducibility (2sigma) of 3-4 permil and 1 percent, respectively. The high sensitivity (> 300 000 cps/ppb) together with low background (Porcupine Seabight (MD01-2463G, Mound Thérèse), indicating a purely interglacial growth of deep-water corals on so-called carbonate mounds over several climate cycles.

  14. Determination of selenomethionine, selenocysteine, and inorganic selenium in eggs by HPLC-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lipiec, Elzbieta; Siara, Grzegorz [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Pau (France); Warsaw University of Technology, Warsaw (Poland); Bierla, Katarzyna; Ouerdane, Laurent; Szpunar, Joanna [CNRS/UPPA, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Pau (France)

    2010-05-15

    A method for the simultaneous determination of selenomethionine (SeMet), selenocysteine (SeCys), and selenite [Se(IV)] in chicken eggs was developed. A sample preparation protocol including defatting, protein denaturation, and carbamidomethylation was optimized in order to achieve complete protein digestion and to avoid SeCys losses. Quantification was carried out by reversed-phase HPLC-inductively coupled plasma mass spectrometry (ICP MS) after quantitative isolation of the selenium-containing fraction by size-exclusion liquid chromatography. The detection limits were 0.06, 0.003, and 0.01 {mu}g g{sup -1} (dry weight) for SeCys, Se(IV) and SeMet, respectively, and the precision was 5-10%. The end products of carbamidomethylation of the different selenium species were identified for the first time by electrospray QTOF MS after custom-designed 2D HPLC purification. Differences in selenium speciation in egg yolk and white were highlighted, the yolk containing more SeCys and the white more SeMet. An insight into selenium bioaccessibility in eggs was obtained by digestion with simulated gastric and gastrointestinal juices and size-exclusion HPLC-ICP MS. (orig.)

  15. Determination of tin isotope ratios in cassiterite by femtosecond laser ablation multicollector inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Schulze, Marie; Ziegerick, Marco; Horn, Ingo; Weyer, Stefan; Vogt, Carla

    2017-04-01

    In comparison to isotope analysis of dissolved samples femtosecond laser ablation multicollector inductively coupled plasma mass spectrometry (fs-LA-MC-ICP-MS) enables precise isotope ratio analyses consuming much less sample material and with a minimum effort in sample preparation. This is especially important for the investigation of valuable historical objects for which visual traces of sampling are unwanted. The present study provides a basis for tin isotope ratio measurements using LA-MC-ICP-MS technique. For this, in house isotope standards had to be defined. Investigations on interferences and matrix effects illustrate that beside Sb only high Te contents (with values above those to be expected in cassiterite) result in a significant shift of the measured tin isotope ratios. This effect can partly be corrected for using natural isotope abundances. However, a natural isotope fractionation of Te cannot be excluded. Tin beads reduced from cassiterite were analysed by laser ablation and after dissolution. It was shown that tin isotope ratios can be determined accurately by using fs-LA-MC-ICP-MS. Furthermore the homogeneity of tin isotope ratios in cassiterite was proven.

  16. [Discussion on diagenesis of Xilingang pluton-constrained by X-ray Fluorescence spectroscopy, plasma mass spectrometry and Raman spectroscopy].

    Science.gov (United States)

    Tang, Yu-Kun; Chen, Guo-Neng; Zhang, Ke; Huang, Hai-Hua

    2013-05-01

    The results on Xilingang pluton, mainly consisting of red beds, granites containing numerous debris of red beds and granites, obtained by X-ray fluorescence spectroscopy, plasma mass spectrometry and Raman spectroscopy show: (1) Xilingang pluton from red beds, granites containing numerous debris of red beds to granites has obvious characteristics of decreasing silicon and alkali content, and rising ignition loss, dark mineral content and oxidation index; (2) Chondrite-normalized REE distribution curves and primitive mantle-normalized spider diagram for trace elements of redbed, granites containing numerous debris of red beds and granites have a good consistency, the distribution characteristics of elements are similar to Nanling transformation-type granite; (3) The value of Raman spectrogram characteristic peak of quartz crystal in Xilingang granite decreased from the center of quartz crystal, and FWHM is steady. According to the above, the authors believe that Xilingang granite formed was related to in-situ melting of red beds and underlying strata and magma consolidation. Volatile components were discharged continuously, and oxidation index decreased gradually in the melting process. In the process of diagenesis, the top of pluton tend to be an ongoing silicon and alkali increase, while TFeO and MgO continue to migrate to bottom, and crystallization environment is a relatively closed and steady system.

  17. Lead concentrations and isotope ratios in street dust determined by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Nageotte, S M; Day, J P

    1998-01-01

    A major source of environmental lead, particularly in urban areas, has been from the combustion of leaded petrol. Street dust has previously been used to assess urban lead contamination, and the dust itself can also be a potential source of lead ingestion, particularly to children. The progressive reduction of lead in petrol, in recent years, would be expected to have been reflected in a reduction of lead in urban dust. We have tested this hypothesis by repeating an earlier survey of Manchester street dust and carrying out a comparable survey in Paris. Samples were collected from streets and parks, lead was extracted by digestion with concentrated nitric acid and determined by electrothermal atomic absorption spectrometry. Lead isotope ratios were measured by inductively coupled plasma mass spectrometry. Results for Manchester show that lead concentrations have fallen by about 40% (street dust averages, 941 micrograms g-1 (ppm) in 1975 down to 569 ppm in 1997). In Paris, the lead levels in street dust are much higher and significant differences were observed between types of street (not seen in Manchester). Additionally, lead levels in parks were much lower than in Manchester. Samples collected under the Eiffel Tower had very high concentrations and lead isotope ratios showed that this was unlikely to be fallout from motor vehicles but could be due to the paint used on the tower. Isotope ratios measurements also revealed that lead additives used in France and the UK come from different sources.

  18. Green and Fast Laser Fusion Technique for Bulk Silicate Rock Analysis by Laser Ablation-Inductively Coupled Plasma Mass Spectrometry.

    Science.gov (United States)

    Zhang, Chenxi; Hu, Zhaochu; Zhang, Wen; Liu, Yongsheng; Zong, Keqing; Li, Ming; Chen, Haihong; Hu, Shenghong

    2016-10-18

    Sample preparation of whole-rock powders is the major limitation for their accurate and precise elemental analysis by laser ablation inductively-coupled plasma mass spectrometry (ICPMS). In this study, a green, efficient, and simplified fusion technique using a high energy infrared laser was developed for major and trace elemental analysis. Fusion takes only tens of milliseconds for each sample. Compared to the pressed pellet sample preparation, the analytical precision of the developed laser fusion technique is higher by an order of magnitude for most elements in granodiorite GSP-2. Analytical results obtained for five USGS reference materials (ranging from mafic to intermediate to felsic) using the laser fusion technique generally agree with recommended values with discrepancies of less than 10% for most elements. However, high losses (20-70%) of highly volatile elements (Zn and Pb) and the transition metal Cu are observed. The achieved precision is within 5% for major elements and within 15% for most trace elements. Direct laser fusion of rock powders is a green and notably simple method to obtain homogeneous samples, which will significantly accelerate the application of laser ablation ICPMS for whole-rock sample analysis.

  19. Ultra-performance liquid chromatography-tandem mass spectrometric method for the determination of strychnine and brucine in mice plasma.

    Science.gov (United States)

    Liu, Yanwen; Zhu, Ronghua; Li, Huande; Yan, Miao; Lei, Yanqing

    2011-09-15

    A selective, simple and efficient method-ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for determination of two toxic alkaloids, namely strychnine and brucine in mice plasma. The UPLC separation was carried out using a 1.7 μm BEH C(18) column (50 mm × 2.1 mm) with a mobile phase consisting of methanol:0.1% formic acid (25:75, v/v), hence providing high efficiency, high resolution and excellent peak shape for the analytes and internal standard. The method was validated over the range of 2.48-496.4 ng/ml for strychnine and 2.64-528 ng/ml for brucine, respectively. Intra- and inter-day accuracy ranged from 95.0% to 107.9% for strychnine, 93.4% to 103.3% for brucine, and the precisions were within 13.8%. The extraction recoveries of both the two alkaloids exceed 81.9%. With a simple and minor sample preparation procedure and short run-time (strychnine and brucine in vivo. Copyright © 2011 Elsevier B.V. All rights reserved.

  20. Roxarsone and transformation products in chicken manure: determination by capillary electrophoresis-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Rosal, Charlita G; Momplaisir, Georges-Marie; Heithmar, Edward M

    2005-04-01

    The determination of the animal feed additive roxarsone (3-nitro-4-hydroxyphenylarsonic acid) and six of its possible transformation products (arsenite, arsenate, monomethylarsonate, dimethylarsinate, 3-amino-4-hydroxyphenylarsonic acid, and 4-hydroxyphenylarsonic acid) in chicken manure was investigated using capillary electrophoresis-inductively coupled plasma-mass spectrometry (CE-ICP-MS). Initial method development was conducted using ultraviolet (UV) detection for ruggedness and time efficiency. Separation of these seven arsenic species was effected using a 20 mM phosphate buffer at pH 5.7. The CE-ICP-MS limits of detection in terms of As for each of the species was in the low microg.L(-1) range, corresponding to absolute detection limits in the range 20-70 fg As (based on a 23 nL injection). Overall, the method developed in this study provides high selectivity and low limits of detection (1-3 microg.L(-1) or low-ppb, based on As), uses small sample volume (low nL), and produces minimal wastes.

  1. Determination of cadmium, mercury and lead in coal fly ash by slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Liao, Hsien-Chung; Jiang, Shiuh-Jen

    1999-08-01

    Ultrasonic slurry sampling electrothermal vaporization isotope dilution inductively coupled plasma mass spectrometry (USS-ETV-ID-ICP-MS) has been applied to the determination of Cd, Hg and Pb in coal fly ash samples. Thioacetamide (TAC) was used as the modifier. Since the sensitivities of the elements studied in coal fly ash slurry and aqueous solution were quite different, isotope dilution method was used for the determination of Cd, Hg and Pb in these coal fly ash samples. The isotope ratios of each element were calculated from the peak areas of each injection peak. This method has been applied to the determination of Cd, Hg and Pb in NIST SRM 1633a coal fly ash reference material and a coal fly ash sample collected from Kaohsiung area. Analysis results of reference sample NIST SRM 1633a coal fly ash agreed satisfactorily with the certified values. The other sample determined by isotope dilution and method of standard additions was agreed satisfactorily. Precision was better than 6% for most of the determinations and accuracy was better than 4% with the USS-ETV-ID-ICP-MS method. Detection limits estimated from standard addition curves were in the range of 24-58, 6-28 and 108-110 ng g-1 for Cd, Hg and Pb, respectively.

  2. Determination of As, Mn, Pb and Se in coal by slurry electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Maia, S.M. da; Silva, J.B.B. Da; Curtius, A.J.; Weiz, B.

    2000-07-01

    A method for the determination of trace elements in coal by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS), introducing the sample as a slurry, is proposed. The slurry was prepared by mixing the powdered coal ({lt} 45 {mu}m) with aqueous 5% v/v nitric acid solution in an ultrasonic bath. An ultrasonic probe was used to homogenize the slurry in the autosampler cup just before its introduction into the graphite tube. By introducing 10{mu}L of 4.0 mg mL{sup -1} coal slurry, using 3{mu}g of Pd as a modifier, and a pyrolysis temperature of 600{degree}C, most of the obtained values for four coal reference materials were well within the certified range, using external calibration with aqueous solutions. No carrier had to be added in addition to the palladium modifier. Using a lower slurry concentration of 1.3 mg mL{sup -1} and 2{mu}g of Pd as the modifier, the values obtained for lead were significantly lower than the certified ones. This problem could be solved in part by adding NaCl as a physical carrier, in addition to the palladium, showing that this carrier reduces the differences in the analyte transport from the sample and from the calibration solutions. However, results for most elements, except for arsenic, tended to be a little low even under these conditions, hence, preference was given to the higher slurry concentration.

  3. Arsenic and selenium speciation in coal fly ash extracts by ion chromatography-inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jackson, B.P.; Miller, W.P. [University of Georgia, Aiken, SC (United States). Savannah River Ecology Lab.

    1998-10-01

    Ion chromatography (IC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) was used to determine As(III), As(V), Se(IV), and Se(VI) in aqueous extracts of coal fly ash. Because all species were fully resolved, the resulting chromatograms were obtained by summing signal intensities for m/z 75 + m/z 82. Absolute detection limits of 7.2, 87, 117 and 28 pg for As(III), Se(IV), Se(VI), and As(V) respectively, were obtained corresponding to 0.072, 0.868, 1.174, and 0.284 {mu} gl{sup -1} for 100 {mu} l injection volume. The technique was used to determine the speciation of As and Se in aqueous extracts of 24 coal fly ash samples including NIST SRM 1633 b. The predominant species were As(V) and Se(IV), with As(III) detected in two low pH fly ashes. Extraction of fly ashes at pH 5 altered the concentrations of total soluble As and Se but did not affect the predominant As and Se speciation.

  4. Laser ablation inductively coupled plasma mass spectrometry: a new tool for trace element analysis in ice cores.

    Science.gov (United States)

    Reinhardt, H; Kriews, M; Miller, H; Schrems, O; Lüdke, C; Hoffmann, E; Skole, J

    2001-07-01

    A new method for the detection of trace elements in polar ice cores using laser ablation with subsequent inductively coupled plasma mass spectrometry analysis is described. To enable direct analysis of frozen ice samples a special laser ablation chamber was constructed. Direct analysis reduces the risk of contamination. The defined removal of material from the ice surface by means of a laser beam leads to higher spatial resolution (300-1000 microm) in comparison to investigations with molten ice samples. This is helpful for the detection of element signatures in annual layers of ice cores. The method was applied to the successful determination of traces for the elements Mg, Al, Fe, Zn, Cd, Pb, some rare-earth elements (REE) and minor constituents such as Ca and Na in ice cores. These selected elements serve as tracer elements for certain sources and their element signatures detected in polar ice cores can give hints to climate changes in the past. We report results from measurements of frozen ice samples, the achievable signal intensities, standard deviations and calibration graphs as well as the first signal progression of 205Pb in an 8,000-year-old ice core sample from Greenland. In addition, the first picture of a crater on an ice surface burnt by an IR laser made by cryogenic scanning electron microscopy is presented.

  5. Discovery and validation of plasma biomarkers for major depressive disorder classification based on liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Liu, Xinyu; Zheng, Peng; Zhao, Xinjie; Zhang, Yuqing; Hu, Chunxiu; Li, Jia; Zhao, Jieyu; Zhou, Jingjing; Xie, Peng; Xu, Guowang

    2015-05-01

    Major depressive disorder (MDD) is a debilitating mental disease with a pronounced impact on the quality of life of many people; however, it is still difficult to diagnose MDD accurately. In this study, a nontargeted metabolomics approach based on ultra-high-performance liquid chromatography equipped with quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) was used to find the differential metabolites in plasma samples from patients with MDD and healthy controls. Furthermore, a validation analysis focusing on the differential metabolites was performed in another batch of samples using a targeted approach based on the dynamic multiple reactions monitoring method. Levels of acyl carnitines, ether lipids, and tryptophan pronouncedly decreased, whereas LPCs, LPEs, and PEs markedly increased in MDD subjects as compared with the healthy controls. Disturbed pathways, mainly located in acyl carnitine metabolism, lipid metabolism, and tryptophan metabolism, were clearly brought to light in MDD subjects. The binary logistic regression result showed that carnitine C10:1, PE-O 36:5, LPE 18:1 sn-2, and tryptophan can be used as a combinational biomarker to distinguish not only moderate but also severe MDD from healthy control with good sensitivity and specificity. Our findings, on one hand, provide critical insight into the pathological mechanism of MDD and, on the other hand, supply a combinational biomarker to aid the diagnosis of MDD in clinical usage.

  6. Direct determination of arsenic in fresh and saline waters by electrothermal vaporization inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Conrad Grégoire, D.; de Lourdes Ballinas, Maria

    1997-01-01

    A method is described for the direct determination of arsenic in fresh and saline waters by electrothermal vaporization inductively coupled plasma mass spectrometry. Arsenic could be determined directly in waters containing up to 10 000 μg ml -1 NaCl without interference from the formation of 75ArCl +. For non-saline waters, arsenic was determined directly with the addition to both aqueous calibration standards and samples of 0.1 μg each of Pd and Mg to act as physical carriers. For the analysis of highly saline waters, the use of Pd and Mg chemical modifier served to thermally stabilize arsenic up to a temperature of 1000°C, while the separate addition of 8 mg of ammonium nitrate was used to remove chloride from the sample. This eliminated serious spectral interference on 75As + from 75ArCl +. Although the ArCl + spectral interference was completely eliminated, residual Na co-volatilized with As caused signal suppression, requiring the use of the method of standard additions for calibration. An absolute limit of detection limit for As of 0.069 pg was obtained corresponding to 6.9 pg ml -1 in a 10 μl sample.

  7. Characterization of silver nanoparticles using flow-field flow fractionation interfaced to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Poda, A R; Bednar, A J; Kennedy, A J; Harmon, A; Hull, M; Mitrano, D M; Ranville, J F; Steevens, J

    2011-07-01

    The ability to detect and identify the physiochemical form of contaminants in the environment is important for degradation, fate and transport, and toxicity studies. This is particularly true of nanomaterials that exist as discrete particles rather than dissolved or sorbed contaminant molecules in the environment. Nanoparticles will tend to agglomerate or dissolve, based on solution chemistry, which will drastically affect their environmental properties. The current study investigates the use of field flow fractionation (FFF) interfaced to inductively coupled plasma-mass spectrometry (ICP-MS) as a sensitive and selective method for detection and characterization of silver nanoparticles. Transmission electron microscopy (TEM) is used to verify the morphology and primary particle size and size distribution of precisely engineered silver nanoparticles. Subsequently, the hydrodynamic size measurements by FFF are compared to dynamic light scattering (DLS) to verify the accuracy of the size determination. Additionally, the sensitivity of the ICP-MS detector is demonstrated by fractionation of μg/L concentrations of mixed silver nanoparticle standards. The technique has been applied to nanoparticle suspensions prior to use in toxicity studies, and post-exposure biological tissue analysis. Silver nanoparticles extracted from tissues of the sediment-dwelling, freshwater oligochaete Lumbriculus variegatus increased in size from approximately 31-46nm, indicating a significant change in the nanoparticle characteristics during exposure.

  8. Determination of noble metals in biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry, following cloud point extraction

    Science.gov (United States)

    Andreia Mesquita da Silva, Márcia; Lúcia Azzolin Frescura, Vera; José Curtius, Adilson

    2001-10-01

    A simple separation procedure for noble metals based on cloud point extraction is proposed. The analyte ions in aqueous acidic solution, obtained by the acid digestion of the samples, were complexed with O, O-diethyl-dithiophosphate and Triton X-114 was added as a non-ionic surfactant. By increasing the temperature up to the cloud point, a phase separation occurs, resulting in an aqueous phase and a surfactant-rich phase containing most of the analytes that were complexed. The metals in the surfactant-rich phase were determined by electrothermal vaporization inductively coupled plasma mass spectrometry. The extraction conditions as well as the instrumental parameters were optimized. Enrichment factors ranging from 7 (Rh) to 60 (Pt) and limits of detection from 0.6 (Pt) to 3.0 ng l -1 (Rh) were obtained in the digested samples. The extraction was not efficient for Ir. Among the reference materials analyzed in this work, only one (SRM 2670, urine) presented recommended values for Au and Pt. Due to the non-availability of adequate CRMs, accuracy was assessed by spiking known analyte amounts to the acid digests. Recoveries close to 100% were observed for all the studied elements but Ru. Poor agreement between found and recommended values was observed for non-digested urine sample, probably due to the carrier effect of co-extracted residual matrix components. However, good agreement was reached after urine acid mineralization.

  9. Sequential cloud point extraction of trace elements from biological samples and determination by inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gine, Maria Fernanda; Patreze, Aparecida F.; Silva, Edson L. [Centro de Energia Nuclear na Agricultura (CENA-USP), Piracicaba, SP (Brazil)]. E-mail: mfgine@cena.usp.br; Sarkis, Jorge E.S.; Kakazu, Mauricio H. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2008-07-01

    A two-step sequential cloud point extraction (CPE) of trace elements from small sample volumes of human serum, animal blood, and food diet is proposed to gain analytical information in the analysis by inductively coupled plasma mass spectrometry. The first CPE was attained by adding O,O-diethyldithiophosphate, the non ionic surfactant Triton{sup R} X-114 followed by heating at 40 deg C, centrifugation and cooling at 0 deg C. The resulting surfactant-rich phase was separated to determine Cd, Pb and Cu by isotope dilution. Isotope ratio measurements presented RSD < 0.7%. The residual surfactant-poor phase solution had the pH adjusted in the range 4 to 5 before the chelating reagent, 4-(2-pyridylazo) resorcinol plus surfactant Triton{sup R} X-114 were added followed by the sequence to attain the CPE. Co and Ni were quantified in the second extracted surfactant-rich phases by standard additions method with RSD < 2%. Recoveries from 85 to 96% were obtained for all elements. Analyzing reference materials with certified and recommended values assessed accuracy. (author)

  10. Complexation studies with lanthanides and humic acid analyzed by ultrafiltration and capillary electrophoresis-inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Kautenburger, Ralf; Beck, Horst Philipp

    2007-08-03

    For the long-term storage of radioactive waste, detailed information about geo-chemical behavior of radioactive and toxic metal ions under environmental conditions is necessary. Humic acid (HA) can play an important role in the immobilisation or mobilisation of metal ions due to complexation and colloid formation. Therefore, we investigate the complexation behavior of HA and its influence on the migration or retardation of selected lanthanides (europium and gadolinium as homologues of the actinides americium and curium). Two independent speciation techniques, ultrafiltration and capillary electrophoresis coupled with inductively coupled plasma mass spectrometry (CE-ICP-MS) have been compared for the study of Eu and Gd interaction with (purified Aldrich) HA. The degree of complexation of Eu and Gd in 25 mg l(-1) Aldrich HA solutions was determined with a broad range of metal loading (Eu and Gd total concentration between 10(-6) and 10(-4) mol l(-1)), ionic strength of 10 mM (NaClO4) and different pH-values. From the CE-ICP-MS electropherograms, additional information on the charge of the Eu species was obtained by the use of 1-bromopropane as neutral marker. To detect HA in the ICP-MS and separate between HA complexed and non complexed metal ions in the CE-ICP-MS, we have halogenated the HA with iodine as ICP-MS marker.

  11. Unambiguous characterization of gunshot residue particles using scanning laser ablation and inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Abrego, Zuriñe; Ugarte, Ana; Unceta, Nora; Fernández-Isla, Alberto; Goicolea, M Aranzazu; Barrio, Ramón J

    2012-03-06

    A new method based on scanning laser ablation and inductively coupled plasma-mass spectrometry (LA-ICPMS) for the detection and identification of gunshot residue (GSR) particles from firearms discharges has been developed. Tape lifts were used to collect inorganic residues from skin surfaces. The laser ablation pattern and ICPMS conditions were optimized for the detection of metals present in GSR, such as (121)Sb, (137)Ba, and (208)Pb. Other isotopes ((27)Al, (29)Si, (31)P, (33)S, (35)Cl, (39)K, (44)Ca, (57)Fe, (60)Ni, (63)Cu, (66)Zn, and (118)Sn) were monitored during the ICPMS analyses to obtain additional information to possibly classify the GSR particles as either characteristic of GSR or consistent with GSR. In experiments with real samples, different firearms, calibers, and ammunitions were used. The performed method evaluation confirms that the developed methodology can be used as an alternative to the standard scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) technique, with the significant advantage of drastically reducing the analysis time to less than 66 min.

  12. Imaging Metals in Brain Tissue by Laser Ablation - Inductively Coupled Plasma - Mass Spectrometry (LA-ICP-MS).

    Science.gov (United States)

    Hare, Dominic J; Kysenius, Kai; Paul, Bence; Knauer, Beate; Hutchinson, Robert W; O'Connor, Ciaran; Fryer, Fred; Hennessey, Tom P; Bush, Ashley I; Crouch, Peter J; Doble, Philip A

    2017-01-22

    Metals are found ubiquitously throughout an organism, with their biological role dictated by both their chemical reactivity and abundance within a specific anatomical region. Within the brain, metals have a highly compartmentalized distribution, depending on the primary function they play within the central nervous system. Imaging the spatial distribution of metals has provided unique insight into the biochemical architecture of the brain, allowing direct correlation between neuroanatomical regions and their known function with regard to metal-dependent processes. In addition, several age-related neurological disorders feature disrupted metal homeostasis, which is often confined to small regions of the brain that are otherwise difficult to analyze. Here, we describe a comprehensive method for quantitatively imaging metals in the mouse brain, using laser ablation - inductively coupled plasma - mass spectrometry (LA-ICP-MS) and specially designed image processing software. Focusing on iron, copper and zinc, which are three of the most abundant and disease-relevant metals within the brain, we describe the essential steps in sample preparation, analysis, quantitative measurements and image processing to produce maps of metal distribution within the low micrometer resolution range. This technique, applicable to any cut tissue section, is capable of demonstrating the highly variable distribution of metals within an organ or system, and can be used to identify changes in metal homeostasis and absolute levels within fine anatomical structures.

  13. Role of laser ablation-inductively coupled plasma-mass spectrometry in cultural heritage research: a review.

    Science.gov (United States)

    Giussani, Barbara; Monticelli, Damiano; Rampazzi, Laura

    2009-03-02

    Cultural heritage represents a bridge between the contemporary society and the past populations, and a strong collaboration between archaeologists, art historians and analysts may lead to the decryption of the information hidden in an ancient object. Quantitative elemental compositional data play a key role in solving questions concerning dating, provenance, technology, use and the relationship of ancient cultures with the environment. Nevertheless, the scientific investigation of an artifact should be carried out complying with some important constraints: above all the analyses should be as little destructive as possible and performed directly on the object to preserve its integrity. Laser ablation sampling coupled to inductively coupled plasma-mass spectrometry (LA-ICP-MS) fulfils these requirements exhibiting comparably strong analytical performance in trace element determination. This review intends to show through the applications found in the literature how valuable is the contribution of LA-ICP-MS in the investigation of ancient materials such as obsidian, glass, pottery, human remains, written heritage, metal objects and miscellaneous stone materials. The main issues related to cultural heritage investigation are introduced, followed by a brief description of the features of this technique. An overview of the exploitation of LA-ICP-MS is then presented. Finally, advantages and drawbacks of this technique are critically discussed: the fit for purpose and prospects of the use of LA-ICP-MS are presented.

  14. A provenance study of iron archaeological artefacts by Inductively Coupled Plasma-Mass Spectrometry multi-elemental analysis

    Energy Technology Data Exchange (ETDEWEB)

    Desaulty, Anne-Marie [Laboratoire Pierre Suee CEA - CNRS/UMR 9956 Centre de Saclay, Bat. 637 91191 Gif sur Yvette, Cedex (France); Laboratoire Metallurgies et culture CNRS/UMR 5060 UTBM 90010 Belfort, Cedex (France); Mariet, Clarisse [Laboratoire Pierre Suee CEA - CNRS/UMR 9956 Centre de Saclay, Bat. 637 91191 Gif sur Yvette, Cedex (France)], E-mail: clarisse.mariet@cea.fr; Dillmann, Philippe [Laboratoire Pierre Suee CEA - CNRS/UMR 9956 Centre de Saclay, Bat. 637 91191 Gif sur Yvette, Cedex (France); Laboratoire Metallurgies et culture CNRS/UMR 5060 UTBM 90010 Belfort, Cedex (France); Joron, Jean Louis [Laboratoire Pierre Suee CEA - CNRS/UMR 9956 Centre de Saclay, Bat. 637 91191 Gif sur Yvette, Cedex (France); Institut de Physique du Globe de Paris, Paris VI et Paris VII, 4, place Jussieu 75252 Paris, Cedex 05 (France); Fluzin, Philippe [Laboratoire Metallurgies et culture CNRS/UMR 5060 UTBM 90010 Belfort, Cedex (France)

    2008-11-15

    Raw materials and wastes (i.e. ore, slag and laitier) from ironmaking archaeological sites have been analyzed in order to understand the behavior of the trace elements in the ancient ironmaking processes and to find the significant-most elements to characterize an iron making region. The ICP-MS (Inductively Coupled Plasma Mass Spectrometry) appears to be an excellent technique for this type of studies. The comparison between the ICP-MS results obtained with the Standard Addition method and the INAA (Instrumental Neutron Activation Analyses) results proved that Sc, Co, (Ni), Rb, Cs, Ba, La, Ce, Sm, Eu, Yb, Hf, Th, U contents in the ores, slag and laitiers, and Co and Ni contents in the cast iron can be successfully determined by ICP-MS after wet acid digestion (low detection limits, good sensitivity and precision). By using significant trace element pairs (Yb/Ce, Ce/Th, La/Sc, U/Th, Nb/Y) present in the ores, laitiers and slag, it is possible to discriminate different French ironmaking regions as the Pays de Bray, Lorraine and Pays d'Ouche. These results open the way to further studies on the provenance of iron objects. The comparison between the ICP-MS results obtained with the Standard Calibration Curves method and the INAA results shows that matrices rich in iron, affect the ICP-MS analyses by suppressing the analytes signal. Further studies are necessary to improve understanding matrix effects.

  15. High-resolution laser ablation-inductively coupled plasma-mass spectrometry imaging of cisplatin-induced nephrotoxic side effects.

    Science.gov (United States)

    Van Acker, Thibaut; Van Malderen, Stijn J M; Van Heerden, Marjolein; McDuffie, James Eric; Cuyckens, Filip; Vanhaecke, Frank

    2016-11-16

    Two-dimensional elemental mapping (bioimaging) via laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was performed on 5 μm thick formalin-fixed, paraffin-embedded kidney tissue sections from Cynomolgus monkeys administered with increasing pharmacological doses of cisplatin. Laterally resolved pixels of 1 μm were achieved, enabling elemental analysis on a (sub-)cellular level. Zones of high Pt response were observed in the renal cortex, where proximal tubules are present, the epithelium of which is responsible for partial reabsorption of cisplatin. Histopathological evaluation, of hematoxylin and eosin-stained serial sections, adjacent to the sections probed via LA-ICP-MS, revealed minimal to mild cisplatin-related lesions (<100 μm) in the renal cortex. Necrotic proximal tubules with sloughed epithelial cells in their lumen could be linked directly to the areas with the highest accumulation of cisplatin, indicating a direct link between cellular concentration and toxicity, thereby providing more insight into the mechanisms through which renal damage occurs.

  16. Standard test method for determination of impurities in nuclear grade uranium compounds by inductively coupled plasma mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2010-01-01

    1.1 This test method covers the determination of 67 elements in uranium dioxide samples and nuclear grade uranium compounds and solutions without matrix separation by inductively coupled plasma mass spectrometry (ICP-MS). The elements are listed in Table 1. These elements can also be determined in uranyl nitrate hexahydrate (UNH), uranium hexafluoride (UF6), triuranium octoxide (U3O8) and uranium trioxide (UO3) if these compounds are treated and converted to the same uranium concentration solution. 1.2 The elements boron, sodium, silicon, phosphorus, potassium, calcium and iron can be determined using different techniques. The analyst's instrumentation will determine which procedure is chosen for the analysis. 1.3 The test method for technetium-99 is given in Annex A1. 1.4 The values stated in SI units are to be regarded as standard. 1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish ...

  17. Simultaneous quantitation of atorvastatin and its two active metabolites in human plasma by liquid chromatography/(-) electrospray tandem mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    Pankaj Partani; S. Manaswita Verma; Sanjay Gurule; Arshad Khuroo; Tausif Monif

    2014-01-01

    A sensitive, accurate and selective liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed and validated for the simultaneous quantitation of atorvastatin (AT) and its equipotent hydroxyl metabolites, 2-hydroxy atorvastatin (2-AT) and 4-hydroxy atorvastatin (4-AT), in human plasma. Electrospray ionization (ESI) interface in negative ion mode was selected to improve the selectivity and the sensitivity required for this application. Additionally, a solid phase extraction (SPE) step was performed to reduce any ion-suppression and/or enhancement effects. The separation of all compounds was achieved in less than 6 min using a C18 reverse-phase fused-cores column and a mobile phase, composed of a mixture of 0.005%formic acid in water:acetonitrile:methanol (35:25:40, v/v/v), in isocratic mode at a flow rate of 0.6 mL/min. The method has lower limit of quantitation (LLOQ) of 0.050 ng/mL for all analytes. The method has shown tremendous reproducibility, with intra-and inter-day precision less than 6.6%, and intra- and inter-day accuracy within 74.3% of nominal values, for all analytes, and has proved to be highly reliable for the analysis of clinical samples.

  18. Simultaneous determination of five anti-epilepsy drugs in human plasma using liquid chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    STEFANIE; WeiBig

    2010-01-01

    A new liquid chromatography-mass spectrometry method for the determination of carbamazepine,clonazepam,alprazolam,estazolam and phenytoin in human plasma has been developed by using diazepam as an internal standard.Chromatographic separation was performed on a Zorbax SB-C18 column(30 mm × 2.1 mm,3.5 ?m) with a mobile phase consisting of methanol and aqueous 25 mM ammonium acetate using gradient elution.A diethyl ether extraction method was used for the extraction of five anti-epilepsy drugs.The final extract was injected for analysis by LC-MS/MS.The method was validated within the concentration range of 50-5000 ng mL-1 for five anti-epilepsy drugs.The precision of the assay(RSD%) was less than 10% at all concentration levels within the tested range.The method recoveries for all samples were more than 90%.The results indicate that the method is specific,sensitive and accurate,and suitable to study the pharmacokinetics,to adjust the dosage for individual administration,and to monitor the drug-concentration and drug abuse of the five anti-epilepsy drugs.

  19. Dry ashing of organic rich matrices with palladium for the determination of arsenic using inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Sahayam, A C; Chaurasia, S C; Venkateswarlu, G

    2010-02-19

    A dry ashing procedure is developed for the determination of As in organic rich matrices such as wheat flour, lichen and tobacco leaves. The volatility of As during dry ashing is avoided by the addition of palladium nitrate [Pd(NO(3))(2)]. The recovery of both As(III) and As(V) is found to be near quantitative. The residue after dry ashing is dissolved in nitric acid (HNO(3)) and analysed by inductively coupled plasma-mass spectrometry (ICP-MS). The process blank and limit of detection (LOD) are 11 and 6.6 ng g(-1), respectively. The procedure is applied for the determination of As in certified reference materials namely wheat flour NIST SRM 1567a (National Institute of Standards and Technology Standard Reference Material), lichen BCR CRM 482 (Institute for Reference Materials, European Commission) and Virginia tobacco leaves CTA-VTL-2 (Poland Academy of Sciences). The results obtained by the present procedure are in good agreement with the certified values and also determined after complete dissolution of samples using closed microwave digestion.

  20. Cathodoluminescence, laser ablasion inductively coupled plasma mass spectrometry, electron probe microanalysis and electron paramagnetic resonance analyses of natural sphalerite

    Science.gov (United States)

    Karakus, M.; Hagni, R.D.; Koenig, A.; Ciftc, E.

    2008-01-01

    Natural sphalerite associated with copper, silver, lead-zinc, tin and tungsten deposits from various world-famous mineral deposits have been studied by cathodoluminescence (CL), laser ablasion inductively coupled plasma mass spectrometry (LA-ICP-MS), electron probe microanalysis (EPMA) and electron paramagnetic resonance (EPR) to determine the relationship between trace element type and content and the CL properties of sphalerite. In general, sphalerite produces a spectrum of CL colour under electron bombardment that includes deep blue, turquoise, lime green, yellow-orange, orange-red and dull dark red depending on the type and concentration of trace quantities of activator ions. Sphalerite from most deposits shows a bright yellow-orange CL colour with ??max centred at 585 nm due to Mn2+ ion, and the intensity of CL is strongly dependent primarily on Fe2+ concentration. The blue emission band with ??max centred at 470-490 nm correlates with Ga and Ag at the Tsumeb, Horn Silver, Balmat and Kankoy mines. Colloform sphalerite from older well-known European lead-zinc deposits and late Cretaceous Kuroko-type VMS deposits of Turkey shows intense yellowish CL colour and their CL spectra are characterised by extremely broad emission bands ranging from 450 to 750 nm. These samples are characterised by low Mn (behaviour of sphalerite serves to characterise ore types and help detect technologically important trace elements.

  1. Investigation of early and advanced stages in ovarian cancer using human plasma by differential scanning calorimetry and mass spectrometry.

    Science.gov (United States)

    Kim, Nam Ah; Jin, Jing Hui; Kim, Kyung-Hee; Lim, Dae Gon; Cheong, Heesun; Kim, Yun Hwan; Ju, Woong; Kim, Seung Cheol; Jeong, Seong Hoon

    2016-05-01

    Ovarian cancer is recognized with high mortality due to asymptomatic nature of the disease and difficulties in diagnosing early stage of the cancer. The present study evaluates the use of differential scanning calorimetry (DSC) in differentiating the severity of ovarian cancer from healthy women. 47 diseased women were subdivided into four stages with respect to clinical relevance and severity. Stages I-II were regarded as early stages and stages III-IV were regarded as advanced stages. The two average transition temperatures (T m ) increased with disease severity from 64.84 and 70.32 °C (healthy) to 68.46 and 75.24 °C (stage IV), respectively. T m were increased depending on clinical groups. In addition, the change in heat capacity was also dependent on the disease severity. To further support and investigate the nature of the proposed interactions, matrix assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) analysis is employed. The results suggest the differences in peptide expression between early and advanced stage of ovarian cancer, affected abundant proteins in plasma. The combined DSC and MS approach was supportive in identifying a unique signature of ovarian cancer stages, and demonstrates the potential of DSC as a complementary diagnostic tool in the evaluation of early stage ovarian cancer.

  2. Analysis of Mineral and Heavy Metal Content of Some Commercial Fruit Juices by Inductively Coupled Plasma Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Adriana Dehelean

    2013-01-01

    Full Text Available The presence of potentially toxic elements and compounds in foodstuffs is of intense public interest and thus requires rapid and accurate methods to determine the levels of these contaminants. Inductively coupled plasma mass spectrometry is a powerful tool for the determination of metals and nonmetals in fruit juices. In this study, 21 commercial fruit juices (apple, peach, apricot, orange, kiwi, pear, pineapple, and multifruit present on Romanian market were investigated from the heavy metals and mineral content point of view by ICP-MS. Our obtained results were compared with those reported in literature and also with the maximum admissible limit in drinking water by USEPA and WHO. For Mn the obtained values exceeded the limits imposed by these international organizations. Co, Cu, Zn, As, and Cd concentrations were below the acceptable limit for drinking water for all samples while the concentrations of Ni and Pb exceeded the limits imposed by USEPA and WHO for some fruit juices. The results obtained in this study are comparable to those found in the literature.

  3. Determination of rare earth elements in dust deposited on tree leaves from Greater Cairo using inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Shaltout, Abdallah A; Khoder, M I; El-Abssawy, A A; Hassan, S K; Borges, Daniel L G

    2013-07-01

    This work aims at monitoring the rare earth elements (REEs) and Th in dust deposited on tree leaves collected inside and outside Greater Cairo (GC), Egypt. Inductively coupled plasma mass spectrometry (ICP-MS) was employed. The concentration of REEs in the collected dust samples was found to be in the range from 1 to 60 μg g(-1). The highest concentration of REEs was found in dust samples collected outside GC, in the middle of the Nile Delta. This would refer to the availability of black sands, due to desert wind occurrence during the sample collection, and anthropogenic activities. The limits of detection of the REEs ranged from 0.02 ng g(-1) for Tm to 3 ng g(-1) for Yb. There was an obvious variation in the concentration of REEs inside and outside GC due to variations of natural and anthropogenic sources. Strong correlations among all the REEs were found.

  4. Comparison of selenium determination in liver samples by atomic absorption spectroscopy and inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Miksa, Irina Rudik; Buckley, Carol L; Carpenter, Nancy P; Poppenga, Robert H

    2005-07-01

    Selenium (Se) is an essential trace element that is often deficient in the natural diets of domestic animal species. The measurement of Se in whole blood or liver is the most accurate way to assess Se status for diagnostic purposes. This study was conducted to compare hydride generation atomic absorption spectroscopy (HG-AAS) with inductively coupled plasma-mass spectrometry (ICP-MS) for the detection and quantification of Se in liver samples. Sample digestion was accomplished with magnesium nitrate and nitric acid for HG-AAS and ICP-MS, respectively. The ICP-MS detection was optimized for 82Se with yttrium used as the internal standard and resulted in a method detection limit of 0.12 microg/g. Selenium was quantified by both methods in 310 samples from a variety of species that were submitted to the Toxicology Laboratory at New Bolton Center (Kennett Square, PA) for routine diagnostic testing. Paired measurements for each sample were evaluated by a mean difference plot method. Limits of agreement were used to describe the maximum differences likely to occur between the 2 methods. Results suggest that under the specified conditions ICP-MS can be reliably used in place of AAS for quantitation of tissue Se at or below 2 microg/g to differentiate between adequate and deficient liver Se concentrations.

  5. Rapid determination of (237)Np and plutonium isotopes in urine by inductively-coupled plasma mass spectrometry and alpha spectrometry.

    Science.gov (United States)

    Maxwell, Sherrod L; Culligan, Brian K; Jones, Vernon D; Nichols, Sheldon T; Noyes, Gary W; Bernard, Maureen A

    2011-08-01

    A new rapid separation method was developed for the measurement of plutonium and neptunium in urine samples by inductively-coupled plasma mass spectrometry (ICP-MS) and/or alpha spectrometry with enhanced uranium removal. This method allows separation and preconcentration of plutonium and neptunium in urine samples using stacked extraction chromatography cartridges and vacuum box flow rates to facilitate rapid separations. There is an increasing need to develop faster analytical methods for emergency response samples. There is also enormous benefit to having rapid bioassay methods in the event that a nuclear worker has an uptake (puncture wound, etc.) to assess the magnitude of the uptake and guide efforts to mitigate dose (e.g., tissue excision and chelation therapy). This new method focuses only on the rapid separation of plutonium and neptunium with enhanced removal of uranium. For ICP-MS, purified solutions must have low salt content and low concentration of uranium due to spectral interference of (238)U(1)H(+) on m/z 239. Uranium removal using this method is enhanced by loading plutonium and neptunium initially onto TEVA resin, then moving plutonium to DGA resin where additional purification from uranium is performed with a decontamination factor of almost 1×10(5). If UTEVA resin is added to the separation scheme, a decontamination factor of ~3 × 10(6) can be achieved.

  6. Breakfast, plasma glucose and beta-hydroxybutyrate, body mass index and academic performance in children from Extremadura, Spain.

    Science.gov (United States)

    Torres, M D; Carmona, I; Campillo, C; Pérez, G; Campillo, J E

    2007-01-01

    Nutritional aspects of breakfast, plasma levels of glucose and beta-hydroxybutyrate, body mass index and academic performance have been studied in urban and rural children (Extremadura, Spain). Representative samples of schoolchildren (3 to 12 years old, random cluster-sampling in schools). Children's mean caloric intake with breakfast was 331 kcal. Rural population ingested more carbohydrates (46,9 +/- 12,3% versus 43,3 +/- 13,2% of the total caloric intake) and fewer lipids (40,5 +/- 11,8% versus 43,9 +/- 12,8% of the total caloric intake) than the urban population. Academic performance was significantly better in the children inhabiting the rural zone than in those of the urban zone. The glycaemia was higher in the urban than in the rural children, and that the contrary was the case for the beta-hydroxybutyrate values. Neither glucose nor beta-hydroxybutyrate levels were correlated with academic performance values. BMI was significantly increased in the urban versus rural children. The present results emphasize the importance of breakfast and life style in the weight and the academic performance of children.

  7. Comparison of laser ablation and dried solution aerosol as sampling systems in inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Coedo, A G; Padilla, I; Dorado, M T

    2004-12-01

    This paper describes a study designed to determine the possibility of using a dried aerosol solution for calibration in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The relative sensitivities of tested materials mobilized by laser ablation and by aqueous nebulization were established, and the experimentally determined relative sensitivity factors (RSFs) were used in conjunction with aqueous calibration for the analysis of solid steel samples. To such a purpose a set of CRM carbon steel samples (SS-451/1 to SS-460/1) were sampled into an ICP-MS instrument by solution nebulization using a microconcentric nebulizer with membrane desolvating (D-MCN) and by laser ablation (LA). Both systems were applied with the same ICP-MS operating parameters and the analyte signals were compared. The RSF (desolvated aerosol response/ablated solid response) values were close to 1 for the analytes Cr, Ni, Co, V, and W, about 1.3 for Mo, and 1.7 for As, P, and Mn. Complementary tests were carried out using CRM SS-455/1 as a solid standard for one-point calibration, applying LAMTRACE software for data reduction and quantification. The analytical results are in good agreement with the certified values in all cases, showing that the applicability of dried aerosol solutions is a good alternative calibration system for laser ablation sampling.

  8. Simultaneous determination of irbesartan and hydrochlorothiazide in human plasma by ultra high performance liquid chromatography tandem mass spectrometry and its application to a bioequivalence study.

    Science.gov (United States)

    Qiu, Xiangjun; Wang, Zhe; Wang, Bing; Zhan, Hui; Pan, Xiaofeng; Xu, Ren-ai

    2014-04-15

    An ultra high performance liquid chromatography tandem mass spectrometry (U-HPLC-MS/MS) method was developed and validated to determine irbesartan (IRB) and hydrochlorothiazide (HCTZ) in human plasma simultaneously. Plasma samples were prepared using protein precipitation with acetonitrile, the two analytes and the internal standard losartan were separated on an Acquity U-HPLC BEH C18 column and mass spectrometric analysis was performed using a QTrap5500 mass spectrometer coupled with an electro-spray ionization (ESI) source in the negative ion mode. The MRM transitions of m/z 427.2→206.9 and m/z 296.1→204.9 were used to quantify for IRB and HCTZ, respectively. The linearity of this method was found to be within the concentration range of 5-3000ng/mL for IRB, and 0.5-300ng/mL for HCTZ in human plasma, respectively. The lower limit of quantification (LLOQ) was 5ng/mL and 0.5ng/mL for IRB and HCTZ in human plasma, respectively. The relative standard deviations (RSD) of intra and inter precision were less than 12% for both IRB and HCTZ. The analysis time of per sample was 2.5min. The developed and validated method was successfully applied to a bioequivalence study of IRB (300mg) with HCTZ (12.5mg) tablet in Chinese healthy volunteers (N=20).

  9. Mass spectrometric study on inactivation mechanism of spore-forming bacteria by low-pressure surface-wave excited oxygen plasma

    Science.gov (United States)

    Zhao, Ying; Ogino, Akihisa; Nagatsu, Masaaki

    2011-05-01

    In this letter, the etching phenomena of the spore-forming bacteria by oxygen plasma were investigated by using quadrupole mass spectrometry. The etching by-products of H2O and CO2 were obviously detected during the oxygen plasma irradiation by the multiple ion detection measurement. Inactivation of roughly 106 spores population was achieved under almost the same reduced spore shapes for three different incident microwave powers. It is considered from the present results that the oxygen radical etching could cause damage to the germinant receptors located in the inner membrane inevitable for germination of spores, without any damage of the DNA in the cores.

  10. Quantitation of Cotinine and its Metabolites in Rat Plasma and Brain Tissue by Hydrophilic Interaction Chromatography Tandem Mass Spectrometry (HILIC-MS/MS)

    OpenAIRE

    Li, Pei; Beck, Wayne D.; Callahan, Patrick M.; Terry, Alvin V.; Bartlett, Michael G

    2012-01-01

    In this work, we developed a sensitive method to quantify cotinine (COT), norcotinine (NCOT), trans-3′-hydroxycotinine (OHCOT) and cotinine-N-oxide (COTNO) in rat plasma and brain tissue, using solid phase extraction (SPE), hydrophilic interaction liquid chromatography (HILIC) and tandem mass spectrometry (MS/MS). The linear range was 1–100 ng/ml for each analyte in rat plasma and brain homogenate (3–300 ng/g brain tissue). The method was validated with precision within 15% relative standard ...

  11. A Thomson-type mass and energy spectrometer for characterizing ion energy distributions in a coaxial plasma gun operating in a gas-puff mode

    OpenAIRE

    Rieker, G.B.; Poehlmann, F. R.; Cappelli, M. A.

    2013-01-01

    Measurements of ion energy distribution are performed in the accelerated plasma of a coaxial electromagnetic plasma gun operating in a gas-puff mode at relatively low discharge energy (900 J) and discharge potential (4 kV). The measurements are made using a Thomson-type mass and energy spectrometer with a gated microchannel plate and phosphor screen as the ion sensor. The parabolic ion trajectories are captured from the sensor screen with an intensified charge-coupled detector camera. The spe...

  12. Sensitive analysis of blonanserin, a novel antipsychotic agent, in human plasma by ultra-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Ogawa, Tadashi; Hattori, Hideki; Kaneko, Rina; Ito, Kenjiro; Iwai, Masayo; Mizutani, Yoko; Arinobu, Tetsuya; Ishii, Akira; Suzuki, Osamu; Seno, Hiroshi

    2010-01-01

    A rapid and sensitive method for analysis of blonanserin in human plasma by ultra-performance liquid chromatography-tandem mass spectrometry is presented. After pretreatment of a plasma sample by solid-phase extraction, blonanserin was analyzed by the system with a C(18) column. This method gave satisfactory recovery rates, reproducibility, and good linearity of calibration curve in the range of 0.01-10.0 ng/mL for quality control samples spiked with blonanserin. The detection limit was as low as 1 pg/mL. This method seems very useful in forensic and clinical toxicology and pharmacokinetic studies.

  13. Measurements of {beta} or {alpha} emitter long lived radionuclides using inductively coupled plasma mass spectrometry; Dosage a tres bas niveau de radionucleides a longue periode emetteurs {beta} ou {alpha} par spectrometrie de masse a couplage plasma inductif

    Energy Technology Data Exchange (ETDEWEB)

    Provitina, O.

    1993-10-18

    The measurement of long-lived radionuclides is highly important for characterizing nuclear wastes for their later storage. The main techniques are {alpha} spectrometry, {beta} counting and {gamma} spectrometry. The large period of these isotopes leads to low specific activity needing time consuming measurements. Moreover, the radiometric techniques are often limited by problems of interferences involving several steps of pretreatments. Among these steps, the specific extraction with crown ethers is highly selective for the separation of {sup 99}Tc, {sup 129}I and {sup 135}Cs. The radiometric techniques are here replaced by inductively coupled plasma mass spectroscopy (ICP-MS) the advantages of which are: few interferences, sensitivity which does not depend on the radiologic period as compared to radiochemistry. ICP-MS can then measure {sup 237}Np in enriched uranium matrix and reduce by a factor of 4 the sample pretreatment and the duration of the analysis usually performed by {alpha} spectrometry. Another technique, electrothermal vaporization (ETV), is consequently used. Crown ether extraction-ETV-ICP-MS is employed for measuring the long lived radionuclides {sup 99}Tc and {sup 129}I. The conditions of the extraction and the parameters of the ETV and the ICP-MS are studied and optimized. The methods optimized (extraction, electrothermal vaporization) are validated in the case of {sup 99}Tc, in real samples. The spike method is required to quantify technetium, the quantification with calibration leading to bad results. The results obtained are in good agreement with the expected values. Extraction of technetium on anionic resin and its measurement by the spike method with pneumatic nebulization-ICP-MS is also performed on other samples. Measured values are also in agreement with expected values, but the method of extraction is more time consuming (half a day) than the extraction with crown ether (one hour). (author). 54 figs., 38 tabs.

  14. Comparison of tunable bandpass reaction cell inductively coupled plasma mass spectrometry with conventional inductively coupled plasma mass spectrometry for the determination of heavy metals in whole blood and urine

    Science.gov (United States)

    Nixon, David E.; Neubauer, Kenneth R.; Eckdahl, Steven J.; Butz, John A.; Burritt, Mary F.

    2004-09-01

    A Dynamic Reaction Cell™ inductively coupled plasma mass spectrometer (DRC-ICP-MS) was evaluated for the determination of arsenic, lead, cadmium, mercury, and thallium in urine and whole blood. Reaction cell conditions were evaluated for suppression of ArCl + and CaCl + polyatomic interferences. The reaction gas was 5% hydrogen in argon. Lead, cadmium, mercury, and thallium were determined with the reaction cell vented. Mixture of 2.5% t-butanol, 0.5% HCl, and 2 mg Au/l plus Ga, Rh, and Bi internal standards was used to dilute whole blood and urine. Calibration was achieved using aqueous acidic standards spiked into urine matrix. Urine and whole blood addition calibration curves were nearly identical for all five elements. DRC-ICP-MS detection limits were equivalent or better than conventional ICP-MS. Within run coefficients of variation (CV's) were nearly the same for DRC-ICP-MS and conventional ICP-MS for National Institute of Standards and Technology (NIST) SRM 2670 and BioRad Lyphochek Urine Metals Control. DRC-ICP-MS within run CV's for As, Pb, Cd, and Hg were 1.9%, 4%, 1.7%, and 1.7%, respectively, for NIST 2670 and 2.9%, 1.8%, 3.4%, 1.7%, and 1.0% for BioRad urine. BioRad Lyphochek Whole Blood control concentrations and CV's were: 78 μg/l (3.8%), 284 μg/l (0.52%), and 544 μg/l (0.9%). With the exception of mercury day-to-day CV's for certified whole blood and urine controls were less than 4% on both the DRC-ICP-MS and conventional ICP-MS.

  15. Atomic structure under external confinement: effect of plasma on the spin orbit splitting, relativistic mass correction and Darwin term for hydrogen-like ions

    Science.gov (United States)

    Chaudhuri, Supriya K.; Mukherjee, Prasanta K.; Fricke, Burkhard

    2017-03-01

    The effect of Debye and quantum plasma environment on the structural properties such as spin orbit splitting, relativistic mass correction and Darwin term for a few iso-electronic members of hydrogen viz. C5 +, O7 +, Ne9 +, Mg11 +, Si13 +, S15 +, Ar17 +, Ca19 + and Ti21 + has been analysed systematically for the first time for a range of coupling strengths of the plasma. The Debye plasma environment has been treated under a standard screened Coulomb potential (SCP) while the quantum plasma has been treated under an exponential cosine screened Coulomb potential (ECSCP). Estimation of the spin orbit splitting under SCP and ECSCP plasma is restricted to the lowest two dipole allowed states while for the other two properties, the ground state as well as the first two excited states have been chosen. Calculations have been extended to nuclear charges for which appreciable relativistic corrections are noted. In all cases calculations have been extended up to such screening parameters for which the respective excitation energies tend towards their stability limit determined by the ionisation potential at that screening parameter. Interesting behavior of the respective properties with respect to the plasma coupling strength has been noted.

  16. Cloud-point extraction is compatible with liquid chromatography coupled to electrospray ionization mass spectrometry for the determination of antazoline in human plasma.

    Science.gov (United States)

    Giebułtowicz, Joanna; Kojro, Grzegorz; Piotrowski, Roman; Kułakowski, Piotr; Wroczyński, Piotr

    2016-09-05

    Cloud-point extraction (CPE) is attracting increasing interest in a number of analytical fields, including bioanalysis, as it provides a simple, safe and environmentally-friendly sample preparation technique. However, there are only few reports on the application of this extraction technique in liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) analysis. In this study, CPE was used for the isolation of antazoline from human plasma. To date, only one method of antazoline isolation from plasma exists-liquid-liquid extraction (LLE). The aim of this study was to prove the compatibility of CPE and LC-ESI-MS/MS and the applicability of CPE to the determination of antazoline in spiked human plasma and clinical samples. Antazoline was isolated from human plasma using Triton X-114 as a surfactant. Xylometazoline was used as an internal standard. NaOH concentration, temperature and Triton X-114 concentration were optimized. The absolute matrix effect was carefully investigated. All validation experiments met international acceptance criteria and no significant relative matrix effect was observed. The compatibility of CPE and LC-ESI-MS/MS was confirmed using clinical plasma samples. The determination of antazoline concentration in human plasma in the range 10-2500ngmL(-1) by the CPE method led to results which are equivalent to those obtained by the widely used liquid-liquid extraction method.

  17. Simultaneous detection of five one-carbon metabolites in plasma using stable isotope dilution liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Adaikalakoteswari, Antonysunil; Webster, Craig; Goljan, Ilona; Saravanan, Ponnusamy

    2016-02-15

    Disturbance in one-carbon (1-C) cycle occurs due to nutritional deficiencies (vitamin B12/folate) or specific genetic polymorphisms. This leads to altered levels of key 1-C metabolites such as SAM (s-adenosyl methionine), SAH (s-adenosyl homocysteine), methionine, homocysteine and MMA (methyl malonic acid). These 1-C metabolites are determinants of cellular methylation potential and epigenetic modifications of DNA which impairs metabolic pathways in several pathological diseases and developmental programming. Though methods were able to measure these analytes only independently, none of the methods detect simultaneously. Therefore we developed a method to measure these five 1-C metabolites in a single run using liquid chromatography tandem mass spectrometry (LC-MS/MS). We used stable isotopes dilution LC-MS/MS to measure the 1-C metabolites in human plasma. Blood samples were collected from pregnant women (n=30) at early gestation in the ongoing, multicentre, prospective PRiDE study. Linearity exhibited across the calibration range for all the analytes with the limit of detection (LOD) of 1.005nmol/l for SAM, 0.081nmol/l for SAH, 0.002μmol/l for methionine, 0.046μmol/l for homocysteine and 3.920nmol/l for MMA. The average recovery for SAM was 108%, SAH-110%, methionine-97%, homocysteine-91% and MMA-102%. The inter-assay CV for SAM was 7.3, SAH-5.6%, methionine-3.5%, homocysteine-7.0% and MMA-4.0%. The intra-assay CV for SAM was 8.7%, SAH-4.7%, methionine-5.4%, homocysteine-8.1% and MMA-6.1%. Pregnant women at early gestation with low B12 levels had significantly higher homocysteine, MMA, lower levels of methionine, SAM and SAM:SAH ratio and higher triglycerides. We developed a simple and rapid method to simultaneously quantify 1-C metabolites such as SAM, SAH, methionine, homocysteine and MMA in plasma by stable isotope dilution LC-MS/MS which would be useful to elucidate the epigenetic mechanisms related in the gene-nutrient interactions.

  18. Plasma bile acids show a positive correlation with body mass index and are negatively associated with cognitive restraint of eating in obese patients

    Science.gov (United States)

    Prinz, Philip; Hofmann, Tobias; Ahnis, Anne; Elbelt, Ulf; Goebel-Stengel, Miriam; Klapp, Burghard F.; Rose, Matthias; Stengel, Andreas

    2015-01-01

    Bile acids may be involved in the regulation of food intake and energy metabolism. The aim of the study was to investigate the association of plasma bile acids with body mass index (BMI) and the possible involvement of circulating bile acids in the modulation of physical activity and eating behavior. Blood was obtained in a group of hospitalized patients with normal weight (BMI 18.5–25 kg/m2), underweight (anorexia nervosa, BMI 50 kg/m2, n = 14–15/group) and plasma bile acid concentrations assessed. Physical activity and plasma bile acids were measured in a group of patients with anorexia nervosa (BMI 14.6 ± 0.3 kg/m2, n = 43). Lastly, in a population of obese patients (BMI 48.5 ± 0.9 kg/m2, n = 85), psychometric parameters related to disordered eating and plasma bile acids were assessed. Plasma bile acids showed a positive correlation with BMI (r = 0.26, p = 0.03) in the population of patients with broad range of BMI (9–85 kg/m2, n = 74). No associations were observed between plasma bile acids and different parameters of physical activity in anorexic patients (p > 0.05). Plasma bile acids were negatively correlated with cognitive restraint of eating (r = −0.30, p = 0.008), while no associations were observed with other psychometric eating behavior-related parameters (p > 0.05) in obese patients. In conclusion, these data may point toward a role of bile acids in the regulation of body weight. Since plasma bile acids are negatively correlated with the cognitive restraint of eating in obese patients, this may represent a compensatory adaptation to prevent further overeating. PMID:26089773

  19. Plasma bile acids show a positive correlation with body mass index and are negatively associated with cognitive restraint of eating in obese patients

    Directory of Open Access Journals (Sweden)

    Philip ePrinz

    2015-06-01

    Full Text Available Bile acids may be involved in the regulation of food intake and energy metabolism. The aim of the study was to investigate the association of plasma bile acids with body mass index (BMI and the possible involvement of circulating bile acids in the modulation of physical activity and eating behavior. Blood was obtained in a group of hospitalized patients with normal weight (BMI 18.5-25 kg/m2, underweight (anorexia nervosa, BMI 50 kg/m2, n=14-15/group and plasma bile acid concentrations assessed. Physical activity and plasma bile acids were measured in a group of patients with anorexia nervosa (BMI 14.6±0.3 kg/m2, n=43. Lastly, in a population of obese patients (BMI 48.5±0.9 kg/m2, n=85, psychometric parameters related to disordered eating and plasma bile acids were assessed. Plasma bile acids showed a positive correlation with BMI (r=0.26, p=0.03 in the population of patients with broad range of BMI (9-85 kg/m2, n=74. No associations were observed between plasma bile acids and different parameters of physical activity in anorexic patients (p>0.05. Plasma bile acids were negatively correlated with cognitive restraint of eating (r=-0.30, p=0.008, while no associations were observed with other psychometric eating behavior-related parameters (p>0.05 in obese patients. In conclusion, these data may point towards a role of bile acids in the regulation of body weight. Since plasma bile acids are negatively correlated with the cognitive restraint of eating in obese patients, this may represent a compensatory adaptation to prevent further overeating.

  20. Determination of metformin in mouse, rat, dog and human plasma samples by laser diode thermal desorption/atmospheric pressure chemical ionization tandem mass spectrometry.

    Science.gov (United States)

    Swales, John G; Gallagher, Richard; Peter, Raimund M

    2010-11-02

    A simple, rapid and robust high-throughput assay for the quantitative analysis of metformin in plasma from different species using laser diode thermal desorption interfaced with atmospheric chemical pressure ionization tandem mass spectrometry (LDTD-APCI-MSMS) was developed for use in a pharmaceutical discovery environment. In order to minimize sample preparation a generic protein precipitation method was used to extract metformin from the plasma. Laser diode thermal desorption is a relatively new sample introduction method, the optimization of the instrumental parameters are presented. The method was successfully applied to spiked mouse, rat, dog and human plasma samples and was subsequently used to determine the oral pharmacokinetics of metformin after dosing to male rats in order to support drug discovery projects. The deviations for intra-assay accuracy and precision across the four species were less than 30% at all calibration and quality control levels.

  1. Quantitation of Cotinine and its Metabolites in Rat Plasma and Brain Tissue by Hydrophilic Interaction Chromatography Tandem Mass Spectrometry (HILIC-MS/MS)

    Science.gov (United States)

    Li, Pei; Beck, Wayne D.; Callahan, Patrick M.; Terry, Alvin V.; Bartlett, Michael G.

    2014-01-01

    In this work, we developed a sensitive method to quantify cotinine (COT), norcotinine (NCOT), trans-3′-hydroxycotinine (OHCOT) and cotinine-N-oxide (COTNO) in rat plasma and brain tissue, using solid phase extraction (SPE), hydrophilic interaction liquid chromatography (HILIC) and tandem mass spectrometry (MS/MS). The linear range was 1–100 ng/ml for each analyte in rat plasma and brain homogenate (3–300 ng/g brain tissue). The method was validated with precision within 15% relative standard deviation (RSD) and accuracy within 15% relative error (RE). Stable isotope-labeled internal standards (IS) were used for all the analytes to achieve good reproducibility, minimizing the influence of recovery and matrix effects. This method can be used in future studies to simultaneously determine the concentrations of COT and three major metabolites in rat plasma and brain tissue. PMID:23022114

  2. Determination of picomolar beryllium levels in seawater with inductively coupled plasma mass spectrometry following silica-gel preconcentration

    Energy Technology Data Exchange (ETDEWEB)

    Tazoe, Hirofumi, E-mail: tazoe@cc.hirosaki-u.ac.jp [Department of Radiation Chemistry, Institute of Radiation Emergency Mediation, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori 036-8564 (Japan); College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Yamagata, Takeyasu [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Obata, Hajime [Atmosphere and Ocean Research Institute, The Tokyo University, 5-1-5 Kashiwanoha, Kashiwa-shi, Chiba 277-8564 (Japan); Nagai, Hisao [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan)

    2014-12-10

    Highlights: • We developesd the simplest and robust SPE method for ultra low picomolar level beryllium in seawater. • Just silica gel column can quantitatively adsorb beryllium in neutral pH condition containing natural seawater. • EDTA solution can eliminate seawater matrixes retaining Be in the column, which optimize to ICP-MS detemination. • Accurate and precise Be data have been obtained for natural seawater from North Pacific Ocean. - Abstract: A robust and rapid method for the determination of natural levels of beryllium (Be) in seawater was developed to facilitate mapping Be concentrations in the ocean. A solid-phase extraction method using a silica gel column was applied for preconcentration and purification of Be in seawater prior to determination of Be concentrations with inductively coupled plasma mass spectrometry (ICP-MS). Be was quantitatively adsorbed onto silica gel from solutions with pH values ranging from 6.3 to 9, including natural seawater. The chelating agent ethylenediamine tetraacetic acid was used to remove other ions in the seawater matrix (Na, Mg, and Ca) that interfere with the ICP-MS analysis. The reproducibility of the method was 3% based on triplicate analyses of natural seawater samples, and the detection limit was 0.4 pmol kg{sup −1} for 250 mL of seawater, which is sufficient for the analysis of seawater in the open ocean. The method was then used to determine the vertical profile of Be in the eastern North Pacific Ocean, which was found to be a recycled-type profile in which the Be concentration increased with depth from the surface (7.2 pmol kg{sup −1} at <200 m) to deep water (29.2 pmol kg{sup −1} from 3500 m to the bottom)

  3. A rapid method for simultaneous determination of arsenic, cadmium and lead in drinking water by inductively coupled plasma mass spectrometry

    Directory of Open Access Journals (Sweden)

    Joshua Rey P. Torres

    Full Text Available The raw water source of drinking water in most areas in the Philippines is typically river water and in some cases groundwater. These sources are prone to elevated levels of metals and metalloids that may cause exposure of the general population when the treatment of the water is inadequate. This work presents a simple method based on EPA Method 200.8 for the determination of total concentrations of arsenic (As, cadmium (Cd and lead (Pb in drinking water using inductively coupled plasma-mass spectrometry (ICP-MS as the element-selective detector. This was applied in the determination of these elements in the water supply in Metro Manila, Philippines. The method detection limits were 0.095 μg L-1, 0.043 μg L-1, and 0.114 μg L-1 for total As, Cd and Pb, respectively.The method was validated using National Institute of Standards and Technology (NIST 1643e certified reference material for trace elements in water and determined values were 60.4 ± 0.5 μg L-1, 6.7 ± 0.1 μg L-1, and 19.6 ± 0.5 μg L-1 for As, Cd and Pb, respectively. These determined values were in good agreement with the certified values in the reference material. Analysis of actual drinking water samples showed that most samples did not exceed the limit of the Philippine drinking water standard for the elements.

  4. Speciation of gadolinium in surface water samples and plants by hydrophilic interaction chromatography hyphenated with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Lindner, Uwe; Lingott, Jana; Richter, Silke; Jakubowski, Norbert; Panne, Ulrich

    2013-02-01

    Hydrophilic interaction chromatography (HILIC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) was optimized for speciation analysis of gadolinium-based contrast agents in environmental samples, in particular surface river waters and plants. Surface water samples from the Teltow channel, near Berlin, were investigated over a distance of 5 km downstream from the influx of a wastewater treatment plant. The total concentration of gadolinium increased significantly from 50 to 990 ng L(-1) due to the influx of the contrast agents. After complete mixing with the river water, the concentration remained constant over a distance of at least 4 km. Two main substances [Dotarem(®) (Gd-DOTA) and Gadovist(®) (Gd-BT-DO3A)] have been identified in the river water using standards. A gadolinium-based contrast agent, possibly Gd-DOTA (Dotarem(®)), was also detected in water plant samples taken from the Teltow channel. Therefore, uptake of contrast agents [Gadovist(®) (Gd-BTDO3A), Magnevist(®) (Gd-DTPA), Omniscan(®) (Gd-DTPA-BMA), Dotarem(®) (Gd-DOTA), and Multihance(®) (Gd-BOPTA)] by plants was investigated in a model experiment using Lepidium sativum (cress plants). HILIC-ICP-MS was used for identification of different contrast agents, and a first approach for quantification using aqueous standard solutions was tested. For speciation analysis, all investigated contrast agents could be extracted from the plant tissues with a recovery of about 54 % for Multihance(®) (Gd-BOPTA) up to 106 % for Gadovist(®) (Gd-BT-DO3A). These experiments demonstrate that all contrast agents investigated are transported from the roots to the leaves where the highest content was measured.

  5. Speciation of cisplatin in environmental water samples by hydrophilic interaction liquid chromatography coupled to inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Vidmar, Janja; Martinčič, Anže; Milačič, Radmila; Ščančar, Janez

    2015-06-01

    Cisplatin is still widely used for treatment of numerous types of tumours. Different speciation methods have been applied to study behaviour of the intact drug and its individual biotransformation species in various clinical samples. These methods are mainly based on electrophoresis, size exclusion (SEC) or ion chromatography (IC) techniques coupled to inductively coupled plasma mass spectrometry (ICP-MS). Hydrophilic interaction liquid chromatography (HILIC), which is a common technique for separation of polar substances, was rarely applied for separation of cisplatin and its hydrolysed metabolites. There is also a lack of information available on the occurrence of cisplatin and its hydrolysed complexes in the environmental waters. In the present study the concentrations of Pt were determined in hospital wastewaters by ICP-MS. A procedure for separation of cisplatin and its aqueous hydrolysed complexes by the use of HILIC column was optimized. Quantification of separated Pt species was performed by isotope dilution (ID)-ICP-MS procedure. Low limits of detection (LODs) and quantification (LOQs) were obtained for cisplatin and its hydrolysed complexes ranging from 0.0273 to 0.1726 ng Pt/mL and from 0.0909 to 0.5753 ng Pt/mL, respectively. Good repeatability of the procedure with relative standard deviation (RSD) lower than ±2.3% was obtained. The column recoveries, which ranged from 95 to 101%, indicated that the procedure developed enabled quantitative speciation analysis of aqueous cisplatin complexes. The ZIC-HILIC-ID-ICP-MS procedure was successfully applied in speciation of cisplatin in spiked hospital wastewater samples.

  6. Simultaneous Determination of Reserpine, Rescinnamine, and Yohimbine in Human Plasma by Ultraperformance Liquid Chromatography Tandem Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Muzaffar Iqbal

    2013-01-01

    Full Text Available A sensitive and selective UPLC-MS/MS method was developed and validated for the determination of three indolic alkaloids (reserpine, rescinnamine, and yohimbine in human plasma using papaverine as internal standard (IS. After a one step protein precipitation with acetonitrile, separation was carried out using C18 column (50 × 2.1 mm, i.d. 1.7 μm and mobile phase consisting of acetonitrile : water : formic acid (60 : 40 : 0.1%, v/v/v pumped at a flow rate of 0.2 mL/min. The mass spectrometric determination was carried out using an electrospray interface operated in the positive mode with multiple reaction monitoring (MRM mode. The precursor to product ion transitions of m/z 609.32 > 195.01, m/z 635.34 > 221.03, m/z 355.19 > 144, and m/z 340.15 > 202.02 were selected for the quantification of reserpine, rescinnamine, yohimbine, and IS, respectively. The analytical response was found to be linear in the range of 0.36–400, 0.27–300, and 0.23–250 ng/mL with lower limit of quantification of 0.36, 0.27, and 0.23 ng/mL for reserpine, rescinnamine, and yohimbine, respectively. Validation was made following official guidelines. The proposed method enabled reproducible results and hence could be reliable for pharmacokinetic and toxicological analysis.

  7. Determination of mercury in coal by isotope dilution cold-vapor generation inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Long, Stephen E; Kelly, W Robert

    2002-04-01

    A method based on isotope dilution cold-vapor inductively coupled plasma mass spectrometry (ID-CV-ICPMS) has been developed for high-accuracy determinations of mercury in bituminous and sub-bituminous coals. A closed-system digestion process employing a Carius tube is used to completely oxidize the coal matrix and chemically equilibrate the mercury in the sample with a 201Hg isotopic spike. The digestates are diluted with high-purity quartz-distilled water, and the mercury is released as a vapor by reduction with tin(II) chloride. Measurements of 201Hg/202Hg isotope ratios are made using a quadrupole ICPMS system in time-resolved analysis mode. The new method has some significant advantages over existing methods. The instrument detection limit is less than 1 pg/mL. The average blank (n = 17) is 30 pg, which is roughly 1 order of magnitude lower than the equivalent microwave digestion procedure. The detection limit in coal is blank limited and is approximately 40 pg/g. Memory effects are very low. The relative reproducibility of the analytical measurements is approximately 0.5% for mercury concentrations in the range 10-150 ng/g. The method has been used to measure mercury concentrations in six coal reference materials, SRM 1632b (77.4 ng/g), SRM 1632c (94.3 ng/g), BCR 40 (433.2 ng/g), BCR 180 (125.0 ng/g), BCR 181 (135.8 ng/g), and SARM 20 (252.6 ng/g), as well as a coal fly ash, SRM 1633b (143.1 ng/g). The method is equally applicable to other types of fossil fuels including both crude and refined oils.

  8. Determination of mercury in coal by isotope dilution cold-vapor generation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Long, S.E.; Kelly, W.R.

    2002-04-01

    A method based on isotope dilution cold-vapor inductively coupled plasma mass spectrometry (ID-CV-ICPMS) has been developed for high-accuracy determinations of mercury in bituminous and sub-bituminous coals. A closed-system digestion process employing a Carius tube is used to completely oxidize the coal matrix and chemically equilibrate the mercury in the sample with a Hg-201 isotopic spike. The digestates are diluted with high-purity quartz-distilled water, and the mercury is released as a vapor by reduction with tin chloride. Measurements of Hg-201/Hg-202 isotope ratios are made using a quadrupole ICPMS system in time-resolved analysis mode. The new method has some significant advantages over existing methods. The instrument detection limit is less than 1 pg/mL. The average blank (n = 17) is 30 pg, which is roughly 1 order of magnitude lower than the equivalent microwave digestion procedure. The detection limit in coal is blank limited and is similar to 40 pg/g. Memory effects are very low. The relative reproducibility of the analytical measurements is similar to 0.5% for mercury concentrations in the range 10-150 ng/g. The method has been used to measure mercury concentrations in six coal reference materials, SRM 1632b (77.4 ng/g), SRM 1632c (94.3 ng/g), BCR 40 (433.2 ng/g), BCR 180 (125.0 ng/g), BCR 181 (135.8 ng/g), and SARM 20 (252.6 ng/g), as well as a coal fly ash, SRM 1633b (143.1 ng/g). The method is equally applicable to other types of fossil fuels including both crude and refined oils.

  9. Multicapillary gas chromatography coupled to inductively coupled plasma-time-of-flight mass spectrometry for rapid mercury speciation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Jitaru, Petru; Goenaga Infante, Heidi; Adams, Freddy C

    2003-08-11

    A simple, rapid and accurate method on the basis of multicapillary gas chromatography (MCGC) combined with inductively coupled plasma-time-of-flight mass spectrometry (ICP-TOFMS) was developed for speciation analysis of methylmercury (MeHg{sup +}) and inorganic mercury (Hg{sup 2+}). The potential of the ICP-TOFMS for transient multi-isotope detection of very short signals (peak width of 0.4 s at half peak height) was evaluated. Two injection systems (purge-and-trap (PTI) and split (SI) injections) were compared in terms of species separation resolution and transient signal profile. Using purge-and-trap injection, after in situ derivatization of the ionic mercury species with sodium tetraethylborate, a baseline separation of MeHg{sup +} and Hg{sup 2+} was achieved within a chromatographic run of <35 s. To correct for matrix-induced ion signal variation and instrumental drift, propylmercury (PrHg{sup +}) was used as internal standard. Detection limits of 16 and 257 fg g{sup -1} for MeHg{sup +} (as Hg) and Hg{sup 2+}, respectively, were achieved. The analytical precision (R.S.D. (%)) for 10 successive injections of a standard mixture containing 10 pg MeHg{sup +} (as Hg) and Hg{sup 2+} was 1.2% for MeHg{sup +} and 4.1% for Hg{sup 2+}. The method was validated by analysis of two biological certified reference materials (CRM): a dogfish muscle (DORM-2) and a freeze-dried tuna fish (CRM 464)

  10. Role of the duodenum in regulation of plasma ghrelin levels and body mass index after subtotal gastrectomy

    Institute of Scientific and Technical Information of China (English)

    Hai-Tao Wang; Qi-Cheng Lu; Qing Wang; Rong-Chao Wang; Yun Zhang; Hai-Long Chen; Hong Zhao; Hai-Xin Qian

    2008-01-01

    AIM: To investigate the role of the duodenum in the regulation of plasma ghrelin levels and body mass index (BMI), and the correlation